Technical Resources

Technical Notes

Technical Notes

 

Oil of Catnip by Supercritical Fluid Extraction

Dr. James Louey, Nathan Petersen, Dennis Salotti, Heather Shaeffer

Chemistry Department, Sacred Heart University 5151 Park Avenue, Fairfield, CT 06432-1000

Dr. Kenneth James, Supercritical Fluid Technologies, Inc. One Innovation Way, Suite 303, Newark, Delaware 19711; Tel: 302-738-3420 x201; Fax: 302-738-4320; E-mail: ken.james@supercriticalfluids.com

 

May 4, 2001

Abstract

Supercritical fluids and in particular supercritical fluid carbon dioxide have shown to be a viable technology for a variety of extractions. While process conditions require high pressures, technological advances have now made it feasible to acquire such equipment for the laboratory. Traditionally, the oil of catnip has been isolated by steam distillation. Working with dried plant material, we have introduced supercritical fluid carbon dioxide as an alternative extraction medium. Results of our work including characterization of the major constituent components will be presented.

Click Here to Download PDF

 


 

Application of Near Critical/Supercritical Solvent

Cleaning Processes

Jonathan A. Peters, The Pennsylvania State University, Applied Research Laboratory, P.O. Box 30, State College, PA 16804; Tel: 814-865-6373; Fax: 814-863-7842; E-mail: PNU@PSU.EDU

Dr. Kenneth James, Supercritical Fluid Technologies, Inc. One Innovation Way, Suite 303, Newark, Delaware 19711; Tel: 302-738-3420 x201; Fax: 302-738-4320; E-mail: ken.james@supercriticalfluids.com

Abstract

Carbon dioxide can be used in its liquid (near critical) or supercritical fluid state as a replacement for conventional cleaning solvents, reducing the pollution associated with the operations that would otherwise require significant amounts of volatile organic compounds, ozone depleting substances, or hazardous air pollutants.

The results of several near critical/supercritical parts cleaning and treatment studies performed at the Applied Research Laboratory are discussed. Near critical/supercritical processing is a commercially viable process for many industrial, electronic and medical device cleaning applications. This applications note will focus on industrial applications such as oxygen-service pressure gauges, fuel and transmission oil filters, and bearings.

Click Here to Download PDF

 


 

Advances in Determining the Solubility, Cloud Point, Swelling and Crystallization Properties of Materials in Supercritical Carbon Dioxide

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc., David Chesney, Ph.D., Michigan Technology University, Jennifer L. Lefler, GlaxoSmithKline

Abstract

Direct, visual observation of materials under supercritical conditions is an important first step in the development and refinement of supercritical fluid extraction, reaction, and chromatographic processes. A specially designed phase equilibrium view cell or “Phase Monitor” is used to observe the dissolution, melting, precipitation, swelling and crystallization of compounds at a wide range of pressures and temperatures. Observations of materials are performed in the supercritical region, under precisely controlled conditions. The Phase Monitor simplifies the determination of critical point for binary, tertiary or complex mixtures. Through a better understanding of phase behavior as a function of temperature, pressure, and sample concentration, a significant time and cost savings for supercritical process development is realized. Examples of the Phase Monitor’s utility are presented.

Click Here to Download PDF

 


 

Assessing Technical Feasibility of Supercritical Extraction Processes of Naturally Occurring Materials Using Benchtop Laboratory Equipment

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc.,

Abstract

The primary goal of a laboratory SFE and Phase Monitor unit testing is to assess technical feasibility of a potential supercritical fluid extraction application. Experimental work begins using a supercritical fluid extraction bench top laboratory unit. The bench scale laboratory extraction unit typically has 10ml to 4 liter sample vessel capacity. Product samples and data from the feasibility testing are used to assess product quality, and to research the following process variables: 1) Preparation of feedstock 2) Extractor conditions 3) Separator conditions. The extract product is analyzed to determine how changes in these parameters change extract yield, concentration, and quality. Phase equilibrium experiments should be carried out to determine the preliminary processing conditions in which the compound of interest solubilizes and precipitates from the supercritical fluid. This information can then be utilized to give a “starting point” to the extraction and separator processing conditions and insight to a commercial scale supercritical fluid extraction system. If the results from preliminary testing are encouraging, process development protocol is followed by proceeding to the next step. Examples demonstrating the use of both laboratory SFE and supercritical fluid phase equilibrium instrument will be shown in this poster.

Click Here to Download PDF

 


 

Supercritical Fluid Technology: Green Chemistry for the 21st Century

Dr. James Louey, Chemistry Department, Sacred Heart University 5151 Park Avenue, Fairfield, CT 06432-1000

Dr. Kenneth James, Supercritical Fluid Technologies, Inc. One Innovation Way, Suite 303, Newark, Delaware 19711; Tel: 302-738-3420 x201; Fax: 302-738-4320; E-mail: ken.james@supercriticalfluids.com

Abstract

Currently, the U. S. produces millions of tons of pollution each year, and spends billions of dollars controlling this pollution.1 This data clearly indicates that sustainable economic growth will require more than end-product environmental monitoring of existing industrial processes. Rather, the worldwide focus on technology development must include new industrial processing methodology that supports pollution prevention at the source. Such a change in production methodology will effect numerous immediate and long-term benefits, including financial, as fewer capital investments will be necessary for future environmental remediation.

Click Here to Download PDF

 


 

Assessing Feasibility of Supercritical Reaction Processes Using Laboratory Equipment

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc.

Kenneth R. Krewson, Supercritical Fluid Technologies, Inc

Abstract

The primary goal of laboratory supercritical fluid reaction unit testing is to assess technical feasibility of a potential supercritical fluid reaction application. Initial screening with a Phase Equilibrium analyzer should be carried out to determine the processing conditions in which the reagents and products of interest solubilize and/or precipitate from the supercritical fluid. Experimentation then moves to the use of a supercritical fluid reaction laboratory unit. The laboratory unit typically has a 50ml to 4 liter reaction vessel fitted with the appropriate reagent addition modules, mixing, flow meters, and sensors. Product samples and data from the feasibility testing are used to assess product quality, and to research process variables such as: 1) Preparation and solubility of reagents 2) Reaction conditions (temperatures, pressures, use of Co-Solvents to enhance reagent or product solubility. 3) Collection conditions. The reaction product is analyzed to determine how changes in these parameters change yield, purity, and economics of the proposed process. This information can then be utilized to fine tune the reaction to maximize key parameters for a commercial scale supercritical fluid reaction process. Examples demonstrating the use of both and laboratory SFR unit and supercritical fluid phase equilibrium instrument will be presented.

Click Here to Download PDF

 


 

New Advances in Supercritical Fluid Extraction for the Quality Control/Quality Assurance Laboratory for Fat Analysis

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc.

Kenneth R. Krewson, Supercritical Fluid Technologies, Inc.,

Abstract

Supercritical fluid extraction has been gaining acceptance in quality control/quality assurance laboratories as a replacement technology for the traditional “organic solvent intensive” fat analysis methods. Conventional methods of fat analysis for baking dough, milk, and chocolate products are time and labor intensive, and require large amounts of hazardous organic solvents. Supercritical fluid extraction using CO2 as a solvent is an alternative method for extraction and isolation of fat content from these products. SFE for baking dough, liquid milk, and chocolate will be explored in this poster using the SFT-100

Extraction Unit and results compared to the traditional solvent intensive methods.

Click Here to Download PDF

 


 

Practical Applications of a “High Pressure” Chemical Reactor for Small Scale Laboratory Synthesis and Process Development

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc.

Kenneth R. Krewson, Supercritical Fluid Technologies, Inc

Abstract

The goal of a high pressure laboratory reaction unit is to assess technical feasibility of pressurized reaction applications such as Catalytic Chemistry, Hydrolysis, Polymerization, Synthesis, and investigate Process Development. The High Pressure Laboratory Reaction Unit typically consists of a 50 ml to 4 liter reaction vessel fitted with the appropriate solvent (CO2, Liquid, or Gas) and reagent addition modules, mixing, heating/cooling, temperature controls, safety features, flow meters, sensors, and controls. Typical Operation conditions for these units are up to 10,000 psi (68.9 MPa) and 350 degrees Celsius.

Product samples and data from the laboratory unit feasibility testing can be used to assess product quality, and to research process variables such as:

1) Preparation and solubility of reagents
2) Reaction conditions (temperatures, pressures, use of Co-Solvents to enhance reactant or product solubility.
3) Collection conditions.

The reaction product is analyzed to determine how changes in these parameters change yield, purity, and economics of the proposed process. This information can then be utilized to fine tune the reaction to maximize key parameters for a commercial scale reaction process or simply be used for repetitive laboratory scale applications. Examples demonstrating the utility of a High Pressure Reaction Unit for traditional organic synthesis and supercritical fluid synthesis are presented.

Click Here to Download the PDF

TN-101 – Oil of Catnip by Supercritical Fluid Extraction

Dr. James Louey, Nathan Petersen, Dennis Salotti, Heather Shaeffer
Chemistry Department, Sacred Heart University 5151 Park Avenue, Fairfield, CT 06432-1000

Dr. Kenneth James, Supercritical Fluid Technologies, Inc. One Innovation Way, Suite 303, Newark, Delaware 19711; Tel: 302-738-3420 x201; Fax: 302-738-4320; E-mail: ken.james@supercriticalfluids.com 

Abstract

Supercritical fluids and in particular supercritical fluid carbon dioxide have shown to be a viable technology for a variety of extractions. While process conditions require high pressures, technological advances have now made it feasible to acquire such equipment for the laboratory. Traditionally, the oil of catnip has been isolated by steam distillation. Working with dried plant material, we have introduced supercritical fluid carbon dioxide as an alternative extraction medium. Results of our work including characterization of the major constituent components will be presented.

Click Here to Download PDF

TN-102 – Application of Near Critical/Supercritical Solvent – Cleaning Processes

Jonathan A. Peters, The Pennsylvania State University, Applied Research Laboratory, P.O. Box 30, State College, PA 16804; Tel: 814-865-6373; Fax: 814-863-7842; E-mail: PNU@PSU.EDU

Dr. Kenneth James, Supercritical Fluid Technologies, Inc. One Innovation Way, Suite 303, Newark, Delaware 19711; Tel: 302-738-3420 x201; Fax: 302-738-4320; E-mail: ken.james@supercriticalfluids.com

Abstract

Carbon dioxide can be used in its liquid (near critical) or supercritical fluid state as a replacement for conventional cleaning solvents, reducing the pollution associated with the operations that would otherwise require significant amounts of volatile organic compounds, ozone depleting substances, or hazardous air pollutants.

The results of several near critical/supercritical parts cleaning and treatment studies performed at the Applied Research Laboratory are discussed. Near critical/supercritical processing is a commercially viable process for many industrial, electronic and medical device cleaning applications. This applications note will focus on industrial applications such as oxygen-service pressure gauges, fuel and transmission oil filters, and bearings.

Click Here to Download PDF

TN-103 – Advances in Determining the Solubility, Cloud Point, Swelling and Crystallization Properties of Materials in Supercritical Carbon Dioxide

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc., David Chesney, Ph.D., Michigan Technology University, Jennifer L. Lefler, GlaxoSmithKline

Abstract

Direct, visual observation of materials under supercritical conditions is an important first step in the development and refinement of supercritical fluid extraction, reaction, and chromatographic processes. A specially designed phase equilibrium view cell or “Phase Monitor” is used to observe the dissolution, melting, precipitation, swelling and crystallization of compounds at a wide range of pressures and temperatures. Observations of materials are performed in the supercritical region, under precisely controlled conditions. The Phase Monitor simplifies the determination of critical point for binary, tertiary or complex mixtures. Through a better understanding of phase behavior as a function of temperature, pressure, and sample concentration, a significant time and cost savings for supercritical process development is realized. Examples of the Phase Monitor’s utility are presented.

Click Here to Download PDF

TN-104 – Assessing Technical Feasibility of Supercritical Extraction Processes of Naturally Occurring Materials Using Benchtop Laboratory Equipment

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc.,

Abstract

The primary goal of a laboratory SFE and Phase Monitor unit testing is to assess technical feasibility of a potential supercritical fluid extraction application. Experimental work begins using a supercritical fluid extraction bench top laboratory unit. The bench scale laboratory extraction unit typically has 10ml to 4 liter sample vessel capacity. Product samples and data from the feasibility testing are used to assess product quality, and to research the following process variables: 1) Preparation of feedstock 2) Extractor conditions 3) Separator conditions. The extract product is analyzed to determine how changes in these parameters change extract yield, concentration, and quality. Phase equilibrium experiments should be carried out to determine the preliminary processing conditions in which the compound of interest solubilizes and precipitates from the supercritical fluid. This information can then be utilized to give a “starting point” to the extraction and separator processing conditions and insight to a commercial scale supercritical fluid extraction system. If the results from preliminary testing are encouraging, process development protocol is followed by proceeding to the next step. Examples demonstrating the use of both laboratory SFE and supercritical fluid phase equilibrium instrument will be shown in this poster.

Click Here to Download PDF

TN-105 – Supercritical Fluid Technology: Green Chemistry for the 21st Century

Dr. James Louey, Chemistry Department, Sacred Heart University 5151 Park Avenue, Fairfield, CT 06432-1000

Dr. Kenneth James, Supercritical Fluid Technologies, Inc. One Innovation Way, Suite 303, Newark, Delaware 19711; Tel: 302-738-3420 x201; Fax: 302-738-4320; E-mail: ken.james@supercriticalfluids.com

Abstract

Currently, the U. S. produces millions of tons of pollution each year, and spends billions of dollars controlling this pollution.1 This data clearly indicates that sustainable economic growth will require more than end-product environmental monitoring of existing industrial processes. Rather, the worldwide focus on technology development must include new industrial processing methodology that supports pollution prevention at the source. Such a change in production methodology will effect numerous immediate and long-term benefits, including financial, as fewer capital investments will be necessary for future environmental remediation.

Click Here to Download PDF

TN-106 – Assessing Feasibility of Supercritical Reaction Processes Using Laboratory Equipment

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc.

Kenneth R. Krewson, Supercritical Fluid Technologies, Inc

Abstract

The primary goal of laboratory supercritical fluid reaction unit testing is to assess technical feasibility of a potential supercritical fluid reaction application. Initial screening with a Phase Equilibrium analyzer should be carried out to determine the processing conditions in which the reagents and products of interest solubilize and/or precipitate from the supercritical fluid. Experimentation then moves to the use of a supercritical fluid reaction laboratory unit. The laboratory unit typically has a 50ml to 4 liter reaction vessel fitted with the appropriate reagent addition modules, mixing, flow meters, and sensors. Product samples and data from the feasibility testing are used to assess product quality, and to research process variables such as: 1) Preparation and solubility of reagents 2) Reaction conditions (temperatures, pressures, use of Co-Solvents to enhance reagent or product

solubility. 3) Collection conditions. The reaction product is analyzed to determine how changes in these parameters change yield, purity, and economics of the proposed process. This information can then be utilized to fine tune the reaction to maximize key parameters for a commercial scale supercritical fluid reaction process. Examples demonstrating the use of both and laboratory SFR unit and supercritical fluid phase equilibrium instrument will be presented.

Click Here to Download PDF

TN-107 – New Advances in Supercritical Fluid Extraction for the Quality Control/Quality Assurance Laboratory for Fat Analysis

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc.

Kenneth R. Krewson, Supercritical Fluid Technologies, Inc.,

Abstract

Supercritical fluid extraction has been gaining acceptance in quality control/quality assurance laboratories as a replacement technology for the traditional “organic solvent intensive” fat analysis methods. Conventional methods of fat analysis for baking dough, milk, and chocolate products are time and labor intensive, and require large amounts of hazardous organic solvents. Supercritical fluid extraction using CO2 as a solvent is an alternative method for extraction and isolation of fat content from these products. SFE for baking dough, liquid milk, and chocolate will be explored in this poster using the SFT-100

Extraction Unit and results compared to the traditional solvent intensive methods.

Click Here to Download PDF

TN-108 – Practical Applications of a “High Pressure” Chemical Reactor for Small Scale Laboratory Synthesis and Process Development

Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc.

Kenneth R. Krewson, Supercritical Fluid Technologies, Inc

Abstract

The goal of a high pressure laboratory reaction unit is to assess technical feasibility of pressurized reaction applications such as Catalytic Chemistry, Hydrolysis, Polymerization, Synthesis, and investigate Process Development. The High Pressure Laboratory Reaction Unit typically consists of a 50 ml to 4 liter reaction vessel fitted with the appropriate solvent (CO2, Liquid, or Gas) and reagent addition modules, mixing, heating/cooling, temperature controls, safety features, flow meters, sensors, and controls. Typical Operation conditions for these units are up to 10,000 psi (68.9 MPa) and 350 degrees Celsius.

Product samples and data from the laboratory unit feasibility testing can be used to assess product quality, and to research process variables such as:

1) Preparation and solubility of reagents
2) Reaction conditions (temperatures, pressures, use of Co-Solvents to enhance reactant or product solubility.
3) Collection conditions.

The reaction product is analyzed to determine how changes in these parameters change yield, purity, and economics of the proposed process. This information can then be utilized to fine tune the reaction to maximize key parameters for a commercial scale reaction process or simply be used for repetitive laboratory scale applications. Examples demonstrating the utility of a High Pressure Reaction Unit for traditional organic synthesis and supercritical fluid synthesis are presented.

Click Here to Download PDF

TN-109 – Beer Hop Extraction

Rudy Baskette, Supercritical Fluid Technologies, Inc

The practice of beer brewing is seven thousand years old and has out survived most of the cultures that drank it. While the ancient Babylonians, Romans, Assyrians, and Incan cultures can no longer partake in the nectar of the gods, striving to brew the best beer is still a prevalent goal.  One of the methods to improve the flavor of a beer is to enhance the intensity of the hops.  Supercritical carbon dioxide hop extraction is a method to obtain hop oil extracts with high concentrations (both yield and purity) and quality (less artifacts).

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TN-110 – Peppermint Oil Extraction

Rudy Baskette, Supercritical Fluid Technologies, Inc

Traditionally, the food industry utilizes steam distillation to extract peppermint oil. Steam distillation processes yield an extract that is a combination of pure and thermally decomposed peppermint oil. The extract from traditional steam distillation results in the familiar peppermint taste you find in peppermint candy.

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TN-111 – Removal of Oils and Waxes from Fabric with SFE

Rudy Baskette, Supercritical Fluid Technologies, Inc

Perchloroethylene (as seen in the figure below) has been the standard dry cleaning solvent for over seven decades. Dry cleaning with perchloroethylene not only leaves a distinctive chemical odor on clothes, but can damage colored clothing, buttons, and beads.  Perchloroethylene is also highly carcinogenic substance.  Perchloroethylene remains in clothes; ergo consistent clothing exposure to perchloroethylene substantially raises levels of the carcinogen.

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TN-112 – Sunflower Oil Extraction

Rudy Baskette, Supercritical Fluid Technologies, Inc

Sunflower seeds contain a high concentration of Vitamin E rich oil.The oil is advantageous for human consumption due to the high vitamin E content and the low amounts of saturated fat. The active component of Sunflower Oil Vitamin E is α-Tocopherol, an antioxidant that defends against ROS (reactive oxygen species). The α-Tocopherol is fat soluble and specifically prevents ROS damage during oxidations of polyunsaturated fatty acids in lipids. 

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TN-113 Chocolate Fat Extraction Using Supercritical Fluids

Rudy Baskette, Supercritical Fluid Technologies, Inc

Dark chocolate bars consist of fat, sugar, and cocoa.  In production, clean roasted cocoa beans are ground and stored in a hanging bag within a heated room.  Cocoa fat drips down; the remaining bagged components are the cocoa powder solids. This is referred to as the Broma method.  This cocoa fat is re-introduced with sugar to the cocoa powder in later stages to produce dark chocolate. 

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TN-114 SC CO2 Determination of Benzophenone Cloud Point

Rudy Baskette, Supercritical Fluid Technologies, Inc

Abstract

Benzophenone is a white crystalline organic substance with a slightly sweet rose geranium scent.  In industry it is typically utilized as a photo-initiator, since it breaks down UV light into free radicals when exposed to light. Benzophenone’s protects a range of products from inks, perfumes, cleaning products, to pharmaceuticals, and soaps. Adding  benzophenone to clear plastic packaging such as food containers prevents UV damage to the contents inside. Benzophenone has also been utilized as biochemical probe to map certain peptide interactions.

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TN-115 SC CO2 Extraction of Microalgae Oils for Biodiesel Production

Rudy Baskette, Supercritical Fluid Technologies, Inc

Abstract

As traditional oil reserves become limited, investigation into alternative energy sources becomes increasingly important.  Microalgae are a versatile, renewable resource.  Certain species can produce large amounts of lipids that can be converted to fatty acid methyl ethers (FAME) for biodiesel.

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