Listing and details on the different elution methods (e.g., EECCC, BECCC, Dual mode, recycling mode) that can be implemented in countercurrent chromatography.
This document provides a summary of a presentation on conductometry. It discusses electrochemical cells, types of electrodes including reference and indicator electrodes. It also describes the Nernst equation and its applications in determining solubility products and for analytical chemistry purposes such as measuring ion concentrations using cell potentials. Electrode types including electrodes of the first, second and third kind are explained along with examples like the silver/silver chloride electrode.
This document summarizes voltammetry, an electrochemical method that uses a three-electrode system to obtain information about analytes. A voltage ramp is applied to the working electrode to reduce ions, while current is measured. Common types of voltammetry include cyclic, square wave, differential pulse, and stripping voltammetry. The working electrode potential is varied over time, while the reference electrode potential remains constant. Voltammetry can be used to determine metal ion concentrations, for wastewater analysis, and in various other applications due to its low detection limits and ability to handle high salt concentrations.
Introduction to electrochemistry 2 by t. haraToru Hara
This document provides an overview of electrochemistry concepts including:
1. Electrochemistry involves redox reactions where electrons are gained or lost at electrode interfaces.
2. Thermodynamics and kinetics control redox reactions based on potential differences and charge/mass transfer limitations.
3. The electric double layer forms at electrode interfaces and can be modeled by the Helmholtz and Stern models.
Voltammetry is a technique where a time-dependent potential is applied to an electrochemical cell and the current is measured as a function of the applied potential. This results in a voltammogram which provides qualitative and quantitative information about redox reactions. The earliest technique was polarography developed in the 1920s. Modern voltammetry uses a three-electrode system with various excitation signals applied. Common techniques include normal pulse polarography, differential pulse polarography, staircase polarography and square wave polarography which have better sensitivity than normal polarography. The shape of the voltammetric wave depends on factors like the reversibility of the redox reaction. The diffusion current occurs at very negative potentials where the reaction rate is controlled by diffusion
Voltammetry techniques are used for analyzing mixtures. Differential pulse polarography uses pulses to provide information on chemical form. Cyclic voltammetry involves sweeping the potential of a working electrode and measuring the current. Stripping voltammetry is a two-step technique that uses electrolytic deposition to preconcentrate metal ions on an electrode, then dissolves the deposit to measure trace metals at low concentrations.
This document discusses the principles and methods of voltammetry and polarography. Some key points:
- Voltammetry measures the current-potential curve during electrolysis using a small amount of sample. Polarography uses a dropping mercury electrode as the working electrode.
- In polarographic analysis, a polarized working electrode and depolarized reference electrode are used. No stirring is used. Only a small amount of analyte undergoes electrolysis.
- The limiting diffusion current is proportional to analyte concentration and can be used for quantitative analysis. The half-wave potential is used for qualitative analysis.
- Factors like temperature, supporting electrolyte composition, and mercury electrode potential affect the limiting diffusion current.
This document discusses various electroanalytical techniques. It begins by introducing electroanalytical techniques and their objectives. It then describes different types of techniques including coulometry, amperometry, voltammetry, polarography, potentiometry, conductometry, and others. It also discusses electrochemical cells, potentials in electroanalytical cells using the Nernst equation, and mass transfer processes like migration, convection, and diffusion.
lecture slide on:
Gibbs free energy and Nernst Equation, Faradaic Processes and Factors Affecting Rates of Electrode Reactions, Potentials and Thermodynamics of Cells, Kinetics of Electrode Reactions, Kinetic controlled reactions,Essentials of Electrode Reactions,BUTLER-VOLMER MODEL FOR THE ONE-STEP, ONE-ELECTRON PROCESS,Current-overpotential curves for the system, Mass Transfer by Migration And Diffusion,MASS-TRANSFER-CONTROLLED REACTIONS,
This document provides a summary of a presentation on conductometry. It discusses electrochemical cells, types of electrodes including reference and indicator electrodes. It also describes the Nernst equation and its applications in determining solubility products and for analytical chemistry purposes such as measuring ion concentrations using cell potentials. Electrode types including electrodes of the first, second and third kind are explained along with examples like the silver/silver chloride electrode.
This document summarizes voltammetry, an electrochemical method that uses a three-electrode system to obtain information about analytes. A voltage ramp is applied to the working electrode to reduce ions, while current is measured. Common types of voltammetry include cyclic, square wave, differential pulse, and stripping voltammetry. The working electrode potential is varied over time, while the reference electrode potential remains constant. Voltammetry can be used to determine metal ion concentrations, for wastewater analysis, and in various other applications due to its low detection limits and ability to handle high salt concentrations.
Introduction to electrochemistry 2 by t. haraToru Hara
This document provides an overview of electrochemistry concepts including:
1. Electrochemistry involves redox reactions where electrons are gained or lost at electrode interfaces.
2. Thermodynamics and kinetics control redox reactions based on potential differences and charge/mass transfer limitations.
3. The electric double layer forms at electrode interfaces and can be modeled by the Helmholtz and Stern models.
Voltammetry is a technique where a time-dependent potential is applied to an electrochemical cell and the current is measured as a function of the applied potential. This results in a voltammogram which provides qualitative and quantitative information about redox reactions. The earliest technique was polarography developed in the 1920s. Modern voltammetry uses a three-electrode system with various excitation signals applied. Common techniques include normal pulse polarography, differential pulse polarography, staircase polarography and square wave polarography which have better sensitivity than normal polarography. The shape of the voltammetric wave depends on factors like the reversibility of the redox reaction. The diffusion current occurs at very negative potentials where the reaction rate is controlled by diffusion
Voltammetry techniques are used for analyzing mixtures. Differential pulse polarography uses pulses to provide information on chemical form. Cyclic voltammetry involves sweeping the potential of a working electrode and measuring the current. Stripping voltammetry is a two-step technique that uses electrolytic deposition to preconcentrate metal ions on an electrode, then dissolves the deposit to measure trace metals at low concentrations.
This document discusses the principles and methods of voltammetry and polarography. Some key points:
- Voltammetry measures the current-potential curve during electrolysis using a small amount of sample. Polarography uses a dropping mercury electrode as the working electrode.
- In polarographic analysis, a polarized working electrode and depolarized reference electrode are used. No stirring is used. Only a small amount of analyte undergoes electrolysis.
- The limiting diffusion current is proportional to analyte concentration and can be used for quantitative analysis. The half-wave potential is used for qualitative analysis.
- Factors like temperature, supporting electrolyte composition, and mercury electrode potential affect the limiting diffusion current.
This document discusses various electroanalytical techniques. It begins by introducing electroanalytical techniques and their objectives. It then describes different types of techniques including coulometry, amperometry, voltammetry, polarography, potentiometry, conductometry, and others. It also discusses electrochemical cells, potentials in electroanalytical cells using the Nernst equation, and mass transfer processes like migration, convection, and diffusion.
lecture slide on:
Gibbs free energy and Nernst Equation, Faradaic Processes and Factors Affecting Rates of Electrode Reactions, Potentials and Thermodynamics of Cells, Kinetics of Electrode Reactions, Kinetic controlled reactions,Essentials of Electrode Reactions,BUTLER-VOLMER MODEL FOR THE ONE-STEP, ONE-ELECTRON PROCESS,Current-overpotential curves for the system, Mass Transfer by Migration And Diffusion,MASS-TRANSFER-CONTROLLED REACTIONS,
This document discusses conductometry, which is a method of analysis based on measuring the electrolytic conductance of a solution. It begins by classifying different electrochemical methods, including conductometry and electrophoresis which do not involve redox reactions. It then discusses key concepts in conductometry such as conductivity, conductance, equivalent conductance, and how various factors like ion nature, temperature, concentration, and electrode size affect conductance. It also provides examples of calculating conductance and equivalent conductance from experimental measurements. Instrumentation for conductometric determination includes a conductance cell and conductivity bridge.
Coulometry and electrogravimetric analysis are analytical techniques that involve completely oxidizing or reducing an analyte through electrolysis. In coulometry, the quantity of electrical charge passed is measured and related to the amount of analyte present. In electrogravimetry, the analyte is converted electrolytically into a product that is weighed to determine the analyte amount. Both techniques are accurate and precise, but require ensuring all current passed results in analyte oxidation/reduction. Controlled-potential coulometry uses a constant potential, while controlled-current coulometry applies a constant current, each with their own experimental considerations to achieve complete analyte conversion.
The document provides information about electroanalytical methods of analysis. It defines electroanalytical methods as techniques that study analytes by measuring potentials or currents in an electrochemical cell containing the analyte. It discusses various types of electroanalytical techniques including potentiometry, voltammetry, and Karl Fischer titration. It provides details on the principles, instrumentation, applications, and advantages of these analytical methods.
This document discusses cyclic voltammetry, which is a type of potentiodynamic electrochemical measurement where the current in an electrochemical cell is measured while the cell's potential is varied linearly with time. It describes the components of a voltammetry system, including the working, reference, and counter electrodes, as well as the supporting electrolyte. It also explains the triangular potential waveform used and defines terms like peak current and peak potential. Examples of using cyclic voltammetry to study the redox reaction of hexacyanoferrate ions and biological redox systems like cytochromes are provided.
1. Polarography is an electroanalytical technique that uses a dropping mercury electrode and measures the current as a function of the applied voltage to determine analyte concentration and properties.
2. Key aspects of polarography include using a polarized indicator electrode such as mercury and an unpolarized reference electrode, operating under diffusion-controlled conditions without stirring, and renewing the mercury surface between measurements.
3. The diffusion current is directly proportional to analyte concentration, allowing quantitative analysis via calibration curves or standard addition. Oxygen interference is eliminated by bubbling nitrogen through the solution.
Potentiometry, voltamemtry and conductometryapeksha40
This document discusses various electroanalytical techniques used in clinical laboratories including potentiometry, voltammetry, conductometry, and coulometry. Potentiometry measures electrical potential differences using ion-selective electrodes or redox electrodes. Voltammetry and amperometry are sensitive techniques that apply a voltage to induce an electrochemical reaction and measure the resulting current. Conductometry measures how well ions conduct electricity. Coulometry determines the amount of an electroactive substance by measuring the charge required for its oxidation or reduction reaction. The NOVA-8 analyzer is highlighted as an example that can test for electrolytes, pH, hematocrit, and other clinical analytes using these electroanalytical methods.
This document discusses various electrochemical techniques including voltammetry and polarography. It describes how voltammetry works by plotting current as a function of applied potential. Polarography uses a mercury working electrode. Different electrode configurations (e.g. solid vs. dropping mercury electrode) and cell designs (e.g. 2-electrode vs. 3-electrode) are discussed. Various factors that influence the measurements including mass transport and potential excitations are also summarized.
Basics of Electrochemistry and Electrochemical MeasurementsHalavath Ramesh
A potentiostat is an electronic instrument that controls the voltage difference between a working electrode and a reference electrode by injecting current through an auxiliary electrode. It is used to apply a potential to an electrochemical cell and measure the resulting current. A potentiostat requires a three-electrode cell with a working electrode, reference electrode, and counter electrode. The working electrode is where the potential is controlled and current is measured. Common reference electrodes include the saturated calomel electrode and silver/silver chloride electrode, which maintain a constant potential. The counter electrode completes the circuit by allowing current to flow out of the cell. Potentiostats are used to study electrochemical reactions and processes.
Potentiometry involves measuring the potential difference between two electrodes under equilibrium conditions. There are two main types of electrodes - reference electrodes that maintain a constant potential, and indicator or working electrodes whose potential varies with ion concentration. Common reference electrodes include the standard hydrogen electrode, saturated calomel electrode, and silver/silver chloride electrode. Indicator electrodes include glass membrane electrodes for measuring pH and ion-selective electrodes that respond selectively to specific ions. Potentiometry is used for pH measurements, ion-selective measurements, and potentiometric titrations.
The Detailed Theory and instrumentation of Both Amperometry and Biamperometric analysis is given with Titration curves and Applications.
Medha Thakur (M.Sc Chemistry)
The earliest voltammetric technique
Heyrovsky invented the original polarographic method in 1922, conventional direct current polarography (DCP).
It employs a dropping mercury electrode (DME) to continuously renew the electrode surface.
Diffusion is the mechanism of mass transport.
When an external potential is applied to a cell
containing a reducing substance such as CdCl2,
The following reaction will occur:
Cd2+ + 2e + Hg = Cd(Hg)
The technique depends on increasing the applied
voltage at a steady rate and simultaneously
record photographically the current-voltage
curve (polarogram)
The apparatus used is called a polarograph .
When an external potential is applied to a cell
containing a reducing substance such as CdCl2,
The following reaction will occur:
Cd2+ + 2e + Hg = Cd(Hg)
The technique depends on increasing the applied
voltage at a steady rate and simultaneously
record photographically the current-voltage
curve (polarogram)
The apparatus used is called a polarograph .
Capillary tube about 10-15cm
Int. diameter of 0.05mm
A vertical distance being maintained betwwen DME and the solution
Drop time of 1-5 seconds
Drop diameter 0.5mm
The supporting electrolyte
is a solution of (KNO3, NaCl, Na3PO4) in which the sample (which must be electroactive) is dissolved.
Function of the supporting electrolyte
It raises the conductivity of the solution.
It carries the bulk of the current so prevent the
migration of electroactive materials to working
electrode.
It may control pH
It may associate with the electroactive solute as
in the complexing of the metal ions by ligands.
This document provides an overview of electrochemical cells. It defines oxidation and reduction reactions and describes how electrons are transferred in these reactions. It explains the basic components and workings of electrolytic cells, which use an external power source to drive non-spontaneous chemical reactions, and galvanic cells, which generate electricity from spontaneous reactions. Reversible and irreversible electrodes are also discussed. Thermodynamics relationships for electrochemical cells are outlined.
Electrochemistry 1 the basic of the basicToru Hara
This document discusses key concepts in electrochemistry including the interface between electrode and electrolyte, thermodynamics and kinetics of electrode reactions, and overpotential. The interface contains an electric double layer consisting of an inner monomolecular layer, an outer diffuse region, and an intermediate layer. Overpotential arises from factors like activation energy needed for electrode reactions, concentration gradients that develop at the electrode surface, and resistance of the electrolyte. Overpotential is composed of ohmic drop, activation overpotential, and diffusion overpotential.
Coulometry is an electrochemical method that measures the current needed to completely oxidize or reduce an analyte. There are two forms: controlled potential and controlled current. Controlled potential coulometry applies a constant potential to ensure 100% current efficiency and quantitative reaction of the analyte without interfering species. The decreasing current over time corresponds to decreasing analyte concentration. Controlled current coulometry passes a constant current, allowing more rapid analysis since current does not decrease over time. The total charge simply equals current multiplied by time. Coulometry provides precise, sensitive, and selective analysis of inorganic and organic compounds and can be adapted to automatic titration methods.
Polarography uses a dropping mercury electrode (DME) to measure the current flowing through an electrochemical cell as a function of the applied potential. A polarogram plots this current versus potential and provides qualitative and quantitative information about species undergoing oxidation or reduction reactions. Jaroslav Heyrovsky invented the polarographic method in 1922 and won the Nobel Prize for his contributions to electroanalytical chemistry. All modern voltammetric methods originate from polarography. The DME provides advantages like a reproducible surface area and the ability to form amalgams with metal ions.
This document discusses conductometry, which is a method of analysis based on measuring the electrolytic conductance of a solution. It begins by classifying different electrochemical methods, including conductometry and electrophoresis which do not involve redox reactions. It then discusses key concepts in conductometry such as conductivity, conductance, equivalent conductance, and how various factors like ion nature, temperature, concentration, and electrode size affect conductance. It also provides examples of calculating conductance and equivalent conductance from experimental measurements. Instrumentation for conductometric determination includes a conductance cell and conductivity bridge.
Coulometry and electrogravimetric analysis are analytical techniques that involve completely oxidizing or reducing an analyte through electrolysis. In coulometry, the quantity of electrical charge passed is measured and related to the amount of analyte present. In electrogravimetry, the analyte is converted electrolytically into a product that is weighed to determine the analyte amount. Both techniques are accurate and precise, but require ensuring all current passed results in analyte oxidation/reduction. Controlled-potential coulometry uses a constant potential, while controlled-current coulometry applies a constant current, each with their own experimental considerations to achieve complete analyte conversion.
The document provides information about electroanalytical methods of analysis. It defines electroanalytical methods as techniques that study analytes by measuring potentials or currents in an electrochemical cell containing the analyte. It discusses various types of electroanalytical techniques including potentiometry, voltammetry, and Karl Fischer titration. It provides details on the principles, instrumentation, applications, and advantages of these analytical methods.
This document discusses cyclic voltammetry, which is a type of potentiodynamic electrochemical measurement where the current in an electrochemical cell is measured while the cell's potential is varied linearly with time. It describes the components of a voltammetry system, including the working, reference, and counter electrodes, as well as the supporting electrolyte. It also explains the triangular potential waveform used and defines terms like peak current and peak potential. Examples of using cyclic voltammetry to study the redox reaction of hexacyanoferrate ions and biological redox systems like cytochromes are provided.
1. Polarography is an electroanalytical technique that uses a dropping mercury electrode and measures the current as a function of the applied voltage to determine analyte concentration and properties.
2. Key aspects of polarography include using a polarized indicator electrode such as mercury and an unpolarized reference electrode, operating under diffusion-controlled conditions without stirring, and renewing the mercury surface between measurements.
3. The diffusion current is directly proportional to analyte concentration, allowing quantitative analysis via calibration curves or standard addition. Oxygen interference is eliminated by bubbling nitrogen through the solution.
Potentiometry, voltamemtry and conductometryapeksha40
This document discusses various electroanalytical techniques used in clinical laboratories including potentiometry, voltammetry, conductometry, and coulometry. Potentiometry measures electrical potential differences using ion-selective electrodes or redox electrodes. Voltammetry and amperometry are sensitive techniques that apply a voltage to induce an electrochemical reaction and measure the resulting current. Conductometry measures how well ions conduct electricity. Coulometry determines the amount of an electroactive substance by measuring the charge required for its oxidation or reduction reaction. The NOVA-8 analyzer is highlighted as an example that can test for electrolytes, pH, hematocrit, and other clinical analytes using these electroanalytical methods.
This document discusses various electrochemical techniques including voltammetry and polarography. It describes how voltammetry works by plotting current as a function of applied potential. Polarography uses a mercury working electrode. Different electrode configurations (e.g. solid vs. dropping mercury electrode) and cell designs (e.g. 2-electrode vs. 3-electrode) are discussed. Various factors that influence the measurements including mass transport and potential excitations are also summarized.
Basics of Electrochemistry and Electrochemical MeasurementsHalavath Ramesh
A potentiostat is an electronic instrument that controls the voltage difference between a working electrode and a reference electrode by injecting current through an auxiliary electrode. It is used to apply a potential to an electrochemical cell and measure the resulting current. A potentiostat requires a three-electrode cell with a working electrode, reference electrode, and counter electrode. The working electrode is where the potential is controlled and current is measured. Common reference electrodes include the saturated calomel electrode and silver/silver chloride electrode, which maintain a constant potential. The counter electrode completes the circuit by allowing current to flow out of the cell. Potentiostats are used to study electrochemical reactions and processes.
Potentiometry involves measuring the potential difference between two electrodes under equilibrium conditions. There are two main types of electrodes - reference electrodes that maintain a constant potential, and indicator or working electrodes whose potential varies with ion concentration. Common reference electrodes include the standard hydrogen electrode, saturated calomel electrode, and silver/silver chloride electrode. Indicator electrodes include glass membrane electrodes for measuring pH and ion-selective electrodes that respond selectively to specific ions. Potentiometry is used for pH measurements, ion-selective measurements, and potentiometric titrations.
The Detailed Theory and instrumentation of Both Amperometry and Biamperometric analysis is given with Titration curves and Applications.
Medha Thakur (M.Sc Chemistry)
The earliest voltammetric technique
Heyrovsky invented the original polarographic method in 1922, conventional direct current polarography (DCP).
It employs a dropping mercury electrode (DME) to continuously renew the electrode surface.
Diffusion is the mechanism of mass transport.
When an external potential is applied to a cell
containing a reducing substance such as CdCl2,
The following reaction will occur:
Cd2+ + 2e + Hg = Cd(Hg)
The technique depends on increasing the applied
voltage at a steady rate and simultaneously
record photographically the current-voltage
curve (polarogram)
The apparatus used is called a polarograph .
When an external potential is applied to a cell
containing a reducing substance such as CdCl2,
The following reaction will occur:
Cd2+ + 2e + Hg = Cd(Hg)
The technique depends on increasing the applied
voltage at a steady rate and simultaneously
record photographically the current-voltage
curve (polarogram)
The apparatus used is called a polarograph .
Capillary tube about 10-15cm
Int. diameter of 0.05mm
A vertical distance being maintained betwwen DME and the solution
Drop time of 1-5 seconds
Drop diameter 0.5mm
The supporting electrolyte
is a solution of (KNO3, NaCl, Na3PO4) in which the sample (which must be electroactive) is dissolved.
Function of the supporting electrolyte
It raises the conductivity of the solution.
It carries the bulk of the current so prevent the
migration of electroactive materials to working
electrode.
It may control pH
It may associate with the electroactive solute as
in the complexing of the metal ions by ligands.
This document provides an overview of electrochemical cells. It defines oxidation and reduction reactions and describes how electrons are transferred in these reactions. It explains the basic components and workings of electrolytic cells, which use an external power source to drive non-spontaneous chemical reactions, and galvanic cells, which generate electricity from spontaneous reactions. Reversible and irreversible electrodes are also discussed. Thermodynamics relationships for electrochemical cells are outlined.
Electrochemistry 1 the basic of the basicToru Hara
This document discusses key concepts in electrochemistry including the interface between electrode and electrolyte, thermodynamics and kinetics of electrode reactions, and overpotential. The interface contains an electric double layer consisting of an inner monomolecular layer, an outer diffuse region, and an intermediate layer. Overpotential arises from factors like activation energy needed for electrode reactions, concentration gradients that develop at the electrode surface, and resistance of the electrolyte. Overpotential is composed of ohmic drop, activation overpotential, and diffusion overpotential.
Coulometry is an electrochemical method that measures the current needed to completely oxidize or reduce an analyte. There are two forms: controlled potential and controlled current. Controlled potential coulometry applies a constant potential to ensure 100% current efficiency and quantitative reaction of the analyte without interfering species. The decreasing current over time corresponds to decreasing analyte concentration. Controlled current coulometry passes a constant current, allowing more rapid analysis since current does not decrease over time. The total charge simply equals current multiplied by time. Coulometry provides precise, sensitive, and selective analysis of inorganic and organic compounds and can be adapted to automatic titration methods.
Polarography uses a dropping mercury electrode (DME) to measure the current flowing through an electrochemical cell as a function of the applied potential. A polarogram plots this current versus potential and provides qualitative and quantitative information about species undergoing oxidation or reduction reactions. Jaroslav Heyrovsky invented the polarographic method in 1922 and won the Nobel Prize for his contributions to electroanalytical chemistry. All modern voltammetric methods originate from polarography. The DME provides advantages like a reproducible surface area and the ability to form amalgams with metal ions.
1. pH-zone refining countercurrent chromatography (CCC) can be used to separate acidic compounds. It utilizes differences in partition coefficients (K values) of analytes between basic (Kbase) and acidic (Kacid) conditions.
2. Key steps include testing Kbase and Kacid values of analytes using different pH solvent systems to determine suitability for separation. A suitable system yields Kbase << 1 and Kacid >> 1.
3. Separation of D&C Orange No. 5 is demonstrated using a diethyl ether-acetonitrile-aqueous ammonium acetate solvent system at basic pH as stationary phase and acidic mobile phase.
This document lists and provides links to various commercially available continuous centrifugal precipitation chromatography (CCS) instruments. It mentions the Pharmatech CCC-1000, Kromaton FCPC-B-D, and CCBiotech bench-top centrifugal precipitation chromatograph models. The technology was invented at NIH and licensed to CCBiotech. It also lists instruments from Armen, Dynamic Extractions, Tauto, AECS, Everseiko. CCS is a process that can continuously fractionate high molecular weight molecules in a salt or solvent gradient applied through a membrane.
This document provides instructions for representing chromatographic data using reciprocal symmetry (ReS) and reciprocal symmetry scaling (ReSS). It explains how to calculate partition coefficients (K) from chromatograms and plot the data in ReS or ReSS format. Guidelines are given for selecting the midline position and adjusting the x-axis to fit the data appropriately. Examples show how these techniques can be used to compare chromatographic methods and solvent systems.
The 9th International CCC Event will be held August 1-3, 2016 at Dominican University in River Forest, Illinois. The event will include conferences on August 1-3 and workshops on July 30-31. Brent Friesen, a Chemistry Professor at Dominican University, is the contact for the event. Countercurrent separation is a type of support-free liquid chromatography that has various instrumentation types including countercurrent chromatography, centrifugal partition chromatography, and droplet countercurrent chromatography. It provides advantages such as minimal sample preparation, high mass resolution, no sample loss, reproducibility, flexibility, and mild separation conditions for sensitive molecules.
The different types of instruments are compared in terms of capacity (column volume), resolution, and duration required for the separation of targeted compounds.
This workshop presentation was prepared by Dr. Friesen (http://www.dom.edu/departments/physicalsciences/faculty/j-brent-friesen).
Future and potential of Countercurrent Chromatography (CCC) from preparative isolation of compounds to the production of Knock-out Extracts.
Can CCC become a mainstream technique?
1. The document provides information about an upcoming conference on solvent system selection for countercurrent chromatography (CCC) to be held in Chicago in August 2016.
2. It discusses various topics that will be covered at the conference including historic and current solvent systems used in CCC, instrumentation, empirical and rational approaches for solvent system selection, and guidelines for selecting solvent-stationary phase combinations.
3. References are provided for papers on selecting solvent systems for natural product separations by CCC and strategies for solvent system selection.
How to perform partitioning experiments to calculate the partition coefficient K, and ultimately identify or selection the optimal solvent system for countercurrent chromatography.
This document discusses standards for calibrating brachytherapy radiation sources. It describes how air-kerma strength is used as the primary standard and how this is measured using free-air chambers. Specifically, it discusses the National Institute of Standards and Technology's free-air chambers used to calibrate low-energy photon-emitting brachytherapy sources such as iodine-125, palladium-103, and cesium-131 seeds. Quality assurance measurements are also outlined such as using well chambers to measure sources and determine anisotropy ratios.
This document provides an overview of high performance liquid chromatography (HPLC). It discusses the basic principles of chromatography and various HPLC modes, including normal phase, reversed phase, ion exchange, and size exclusion chromatography. The document also describes HPLC system components like pumps, injectors, columns, ovens, and detectors. It explains isocratic and gradient elution modes and discusses the instrumentation, functions, and advantages of various HPLC detectors.
Electrolysis of Swine Manure Effluents Using Three Different Electrodes FE-FE...LPE Learning Center
The full proceedings paper is at: http://www.extension.org/72845
The main objective of this research was to investigate the electrochemical oxidation of swine manure effluent obtained from a primary lagoon for reducing organic and inorganic pollutants.
ChemFET fabrication, device physics and sensing mechanismRichard Yang
1. Organic thin-film field-effect transistors (OTFTs) were fabricated and tested for chemical sensing applications. Pulsed gate operation was found to significantly reduce device baseline drift compared to static operation.
2. Charge transport in the organic semiconductor films occurs via multiple trapping and release of charge carriers. Variable temperature measurements showed thermally activated transport, with the activation energy dependent on gate voltage.
3. Exposure to chemical vapors causes a change in device characteristics due to the interaction of adsorbed analyte molecules with the doped organic semiconductor surface layer. This modifies both the surface doping level and trap energies.
1. The document discusses dynamic simulations for operation mode transfer of a micro-turbine generator. It analyzes transient power disturbances that occur when transferring operation modes.
2. It shows significant transient power disturbance is induced when transferring from island mode to grid-connected mode. When two units simultaneously connect to a grid, the impact on both units is even more serious.
3. The degree of impact during a mode transfer is not less than the impact on a traditional synchronous generator undergoing a three-phase fault.
Counter current Extraction Solid phase extraction Gel filtrationPHARMA WORLD
This document provides an overview of counter current extraction, solid phase extraction, and gel filtration chromatography techniques. It discusses the principles, processes, instrumentation, and applications of each technique. Counter current extraction uses a series of tubes to separate mixtures into phases based on solubility differences. Solid phase extraction isolates analytes from samples using adsorption onto a solid phase. Gel filtration separates molecules based on size by allowing larger molecules to pass through column pores. Each technique has advantages for analytical separations and preparative isolation of compounds from complex mixtures.
�A) All analog traces. This
view shows peak values. RMS values may also be displayed.
�B) Controls for going to the beginning or end of a record, as well as nudging forward or backward in time in a record.
�C) Zoom controls
�D) Display controls for analog traces, RMS traces, fundamental waveform display, frequency trace, power trace, power factor trace, phasor diagram, impedance diagram and power diagram.
Super Critical Fluid Separation ProcessAbhimanyu Pal
Hello Guys here is a presentation for you named super critical fluid separation process. It may be useful for third year undergraduate of chemical engg. stream. so have a look ,i hope it may be helpful for your project
Original PNP Transistor 2SB688 B688 8A 120V New ToshibaAUTHELECTRONIC
This document summarizes the specifications and characteristics of the 2SB686 silicon PNP triple diffused power transistor. It is recommended for use in 30-35W high-fidelity audio frequency amplifier output stages as a complement to the 2SD716 transistor. The document provides maximum ratings, electrical characteristics, and graphs of current, voltage, power dissipation and gain over temperature ranges.
This document summarizes continuous renal replacement therapy (CRRT) techniques and clinical applications. It discusses:
1) The physical principles of CRRT including convection, diffusion, and filtration and how they impact solute clearance.
2) The definitions of different CRRT modalities including slow continuous ultrafiltration (SCUF), continuous venovenous hemofiltration (CVVH), hemodialysis (CVVHD), and hemodiafiltration (CVVHDF).
3) The clinical indications for CRRT compared to intermittent hemodialysis, including better hemodynamic stability, uremic and metabolic control, and management of conditions like sepsis and inflammation.
This document provides specifications for ELP series aluminum electrolytic capacitors, including:
- Voltage and capacitance ranges from 16-100V and 470uF-47,000uF
- Temperature range of -40°C to +85°C
- Leakage current, dissipation factor, and impedance ratio specifications
- Requirements for capacitance change, dissipation factor, and leakage current after load life and shelf life testing.
This document provides specifications for ELP series aluminum electrolytic capacitors, including:
- Voltage and capacitance ranges from 16-100V and 470uF-47,000uF
- Temperature range of -40°C to +85°C
- Leakage current, dissipation factor, and impedance ratio specifications
- Requirements for capacitance change, dissipation factor, and leakage current after load life and shelf life testing.
This document provides specifications for ELP series aluminum electrolytic capacitors including:
- Voltage and capacitance ranges from 16-100V and 470uF-47,000uF
- Temperature range of -40°C to +85°C
- Leakage current and dissipation factor specifications
- Load life and shelf life test requirements
- Standard product dimensions and maximum ripple current for different capacitance sizes
This document provides specifications for ELP series aluminum electrolytic capacitors including:
- Voltage and capacitance ranges from 16-100V and 470uF-47,000uF
- Temperature range of -40°C to +85°C
- Leakage current and dissipation factor specifications
- Load life and shelf life test requirements
- Standard product dimensions and maximum ripple current for different capacitance sizes
This document discusses analyzing the variance of multiplexed qPCR systems as a whole rather than individually. It provides examples of calculating variance based on the frequency of particles in a matrix for a multiplex system. This %CV value for the whole system provides clarity on whether to accept or reject sample results, with an acceptance threshold of 10% CV compared to controls. Analyzing the system as a single unit accounts for interactions between targets that analyzing them individually does not.
2006 ASME Power Conference Last Stage Performance Considerations in LP Turbin...Komandur Sunder Raj, P.E.
The document presents a case study analyzing the performance of last stage blades (LSB) on low-pressure turbines under various conditions, including changes in unit rating from power uprates. It includes tables showing the impact of LSB size, end loading, condenser operating range, and 15% power uprates on last stage annulus velocity, exhaust loss, efficiency, output, and other parameters. The study examines 43-inch and 52-inch LSBs on a 1100MWe unit and implications for optimizing last stage performance based on relationships between the turbine and condenser system.
This document describes the development of a method for identifying cyclic dinucleotides (CDNs) in bacterial cultures. The author synthesized 10 variants of CDNs and optimized an LC/MS method using C18 columns to separate and identify the CDNs. Testing on synthetic standards showed good separation and detection of CDNs. The method was then applied to bacterial samples, identifying several known CDNs and detecting potential new ones in various bacteria. The method provides a way to preliminarily identify CDNs and study their roles in bacterial physiology and pathogenesis.
Simulating Membrane Channels, E. Tajkhorshid, Part 2TCBG
This document provides instructions for simulating membrane protein systems. It outlines several steps: 1) constrain the protein and relax the lipids and water, 2) monitor water placement to prevent penetration into hydrophobic clefts, 3) monitor simulation box volume until stabilization is reached, 4) release protein constraints and further equilibrate the system, and 5) switch to production simulations like NPT or NVT when stable volume is reached. The focus is on properly packing lipids and water around the protein during initial equilibration simulations.
This document provides technical specifications for 8 power distribution circuits (TGBT A) in French. It includes information about circuit identifiers, voltage levels, cable types and lengths, protection devices, and load details for various distributed components. Maximum voltage drops, current capacities and protection settings are specified for each circuit element. The document also outlines specifications for 6 additional circuits (TGHQ A) in a similar format.
Similar to Elution methods in Countercurrent Chromatography (20)
How to prepare and share your Raw NMR data along with your publication. Sharing your NMR data will enhance the transparency and reproducibility of structure elucidation while improving the dereplication process. This is a guidance document proposed by the CENAPT team. See also the corresponding website at : https://cenapt.pharm.uic.edu/resource/.
This document combined the microscopic analysis, DNA barcoding results, and phytochemical fingerprints for the botanical identification of the following commercial plant materials: Epimedium sagittatum (leaf powder), Marrubium vulgare (crushed aerial parts), Pausinystalia johimbe (bark powder), Senna alexandrina (leaf powder), Trigonellum foenum-graecum ( seed powder), and Trifolium pratense (crushed aerial parts).
Presentation from Dr. Guy Harris at the annual meeting of the American Society of Pharmacognosy (ASP) in Lexington Kentucky (2018) during the CENAPT/Gilson Workshop on Countercurrent Chromatography.
Workshop presented by Gregoire Audo from Gilson Purification at the annual meeting of the American Society of Pharmacognosy (ASP 2018) in Lexington, Kentucky.
Slides presented at the annual meeting of the American Society of Pharmacognosy, Lexington Kentucky (2018). Compile basic information of the principles of countercurrent separation, choice of solvent systems, and determination of partition coefficient.
Prepared by Drs. Charlotte Simmler, Brent Friesen, Guido Pauli from the Center for Natural Product Technologies (CENAPT)
You will find here all the elements presented by the CENAPT team ( Drs. Guido Pauli and Charlotte Simmler) and pertaining to the NMR workshop at the American Society of Pharmacognosy (ASP 2017, Portland Oregon).
These slides summarize the different steps related to the implementation of quantitative NMR for purity analysis.
More from Center for Natural Product Technologies (7)
Sexuality - Issues, Attitude and Behaviour - Applied Social Psychology - Psyc...PsychoTech Services
A proprietary approach developed by bringing together the best of learning theories from Psychology, design principles from the world of visualization, and pedagogical methods from over a decade of training experience, that enables you to: Learn better, faster!
EWOCS-I: The catalog of X-ray sources in Westerlund 1 from the Extended Weste...Sérgio Sacani
Context. With a mass exceeding several 104 M⊙ and a rich and dense population of massive stars, supermassive young star clusters
represent the most massive star-forming environment that is dominated by the feedback from massive stars and gravitational interactions
among stars.
Aims. In this paper we present the Extended Westerlund 1 and 2 Open Clusters Survey (EWOCS) project, which aims to investigate
the influence of the starburst environment on the formation of stars and planets, and on the evolution of both low and high mass stars.
The primary targets of this project are Westerlund 1 and 2, the closest supermassive star clusters to the Sun.
Methods. The project is based primarily on recent observations conducted with the Chandra and JWST observatories. Specifically,
the Chandra survey of Westerlund 1 consists of 36 new ACIS-I observations, nearly co-pointed, for a total exposure time of 1 Msec.
Additionally, we included 8 archival Chandra/ACIS-S observations. This paper presents the resulting catalog of X-ray sources within
and around Westerlund 1. Sources were detected by combining various existing methods, and photon extraction and source validation
were carried out using the ACIS-Extract software.
Results. The EWOCS X-ray catalog comprises 5963 validated sources out of the 9420 initially provided to ACIS-Extract, reaching a
photon flux threshold of approximately 2 × 10−8 photons cm−2
s
−1
. The X-ray sources exhibit a highly concentrated spatial distribution,
with 1075 sources located within the central 1 arcmin. We have successfully detected X-ray emissions from 126 out of the 166 known
massive stars of the cluster, and we have collected over 71 000 photons from the magnetar CXO J164710.20-455217.
The debris of the ‘last major merger’ is dynamically youngSérgio Sacani
The Milky Way’s (MW) inner stellar halo contains an [Fe/H]-rich component with highly eccentric orbits, often referred to as the
‘last major merger.’ Hypotheses for the origin of this component include Gaia-Sausage/Enceladus (GSE), where the progenitor
collided with the MW proto-disc 8–11 Gyr ago, and the Virgo Radial Merger (VRM), where the progenitor collided with the
MW disc within the last 3 Gyr. These two scenarios make different predictions about observable structure in local phase space,
because the morphology of debris depends on how long it has had to phase mix. The recently identified phase-space folds in Gaia
DR3 have positive caustic velocities, making them fundamentally different than the phase-mixed chevrons found in simulations
at late times. Roughly 20 per cent of the stars in the prograde local stellar halo are associated with the observed caustics. Based
on a simple phase-mixing model, the observed number of caustics are consistent with a merger that occurred 1–2 Gyr ago.
We also compare the observed phase-space distribution to FIRE-2 Latte simulations of GSE-like mergers, using a quantitative
measurement of phase mixing (2D causticality). The observed local phase-space distribution best matches the simulated data
1–2 Gyr after collision, and certainly not later than 3 Gyr. This is further evidence that the progenitor of the ‘last major merger’
did not collide with the MW proto-disc at early times, as is thought for the GSE, but instead collided with the MW disc within
the last few Gyr, consistent with the body of work surrounding the VRM.
The technology uses reclaimed CO₂ as the dyeing medium in a closed loop process. When pressurized, CO₂ becomes supercritical (SC-CO₂). In this state CO₂ has a very high solvent power, allowing the dye to dissolve easily.
When I was asked to give a companion lecture in support of ‘The Philosophy of Science’ (https://shorturl.at/4pUXz) I decided not to walk through the detail of the many methodologies in order of use. Instead, I chose to employ a long standing, and ongoing, scientific development as an exemplar. And so, I chose the ever evolving story of Thermodynamics as a scientific investigation at its best.
Conducted over a period of >200 years, Thermodynamics R&D, and application, benefitted from the highest levels of professionalism, collaboration, and technical thoroughness. New layers of application, methodology, and practice were made possible by the progressive advance of technology. In turn, this has seen measurement and modelling accuracy continually improved at a micro and macro level.
Perhaps most importantly, Thermodynamics rapidly became a primary tool in the advance of applied science/engineering/technology, spanning micro-tech, to aerospace and cosmology. I can think of no better a story to illustrate the breadth of scientific methodologies and applications at their best.
PPT on Direct Seeded Rice presented at the three-day 'Training and Validation Workshop on Modules of Climate Smart Agriculture (CSA) Technologies in South Asia' workshop on April 22, 2024.
Mending Clothing to Support Sustainable Fashion_CIMaR 2024.pdfSelcen Ozturkcan
Ozturkcan, S., Berndt, A., & Angelakis, A. (2024). Mending clothing to support sustainable fashion. Presented at the 31st Annual Conference by the Consortium for International Marketing Research (CIMaR), 10-13 Jun 2024, University of Gävle, Sweden.
Immersive Learning That Works: Research Grounding and Paths ForwardLeonel Morgado
We will metaverse into the essence of immersive learning, into its three dimensions and conceptual models. This approach encompasses elements from teaching methodologies to social involvement, through organizational concerns and technologies. Challenging the perception of learning as knowledge transfer, we introduce a 'Uses, Practices & Strategies' model operationalized by the 'Immersive Learning Brain' and ‘Immersion Cube’ frameworks. This approach offers a comprehensive guide through the intricacies of immersive educational experiences and spotlighting research frontiers, along the immersion dimensions of system, narrative, and agency. Our discourse extends to stakeholders beyond the academic sphere, addressing the interests of technologists, instructional designers, and policymakers. We span various contexts, from formal education to organizational transformation to the new horizon of an AI-pervasive society. This keynote aims to unite the iLRN community in a collaborative journey towards a future where immersive learning research and practice coalesce, paving the way for innovative educational research and practice landscapes.
Describing and Interpreting an Immersive Learning Case with the Immersion Cub...Leonel Morgado
Current descriptions of immersive learning cases are often difficult or impossible to compare. This is due to a myriad of different options on what details to include, which aspects are relevant, and on the descriptive approaches employed. Also, these aspects often combine very specific details with more general guidelines or indicate intents and rationales without clarifying their implementation. In this paper we provide a method to describe immersive learning cases that is structured to enable comparisons, yet flexible enough to allow researchers and practitioners to decide which aspects to include. This method leverages a taxonomy that classifies educational aspects at three levels (uses, practices, and strategies) and then utilizes two frameworks, the Immersive Learning Brain and the Immersion Cube, to enable a structured description and interpretation of immersive learning cases. The method is then demonstrated on a published immersive learning case on training for wind turbine maintenance using virtual reality. Applying the method results in a structured artifact, the Immersive Learning Case Sheet, that tags the case with its proximal uses, practices, and strategies, and refines the free text case description to ensure that matching details are included. This contribution is thus a case description method in support of future comparative research of immersive learning cases. We then discuss how the resulting description and interpretation can be leveraged to change immersion learning cases, by enriching them (considering low-effort changes or additions) or innovating (exploring more challenging avenues of transformation). The method holds significant promise to support better-grounded research in immersive learning.
(June 12, 2024) Webinar: Development of PET theranostics targeting the molecu...Scintica Instrumentation
Targeting Hsp90 and its pathogen Orthologs with Tethered Inhibitors as a Diagnostic and Therapeutic Strategy for cancer and infectious diseases with Dr. Timothy Haystead.
2. elution method phase changea
flow
direction
change
rotation
direction
change
comments
classical – – – highly retained analytes remain in stationary
phase
EECCC single – – analytes elute in order of K values
BECCC – single – elution order reverses; some analytes may
elute at separate volumes
back-step CCC twice – – a plug of aqueous phase introduced to elute
highly retained analytes
dual-mode single single – elution order reverses
dual-rotation single single elution order reverses
multiple dual-mode multiple multiple – elution order reverses each cycle
ICcE multiple multiple – sample loop is in the middle of a single
column or between two separate columns
recycling eluant fraction reintroduced into column
aphase change refers to switching mobile and stationary phase
Countercurrent Separation Elution Methods
Friesen JB, McAlpine JB, Chen SN, Pauli GF
Countercurrent Separation of Natural Products: An Update
Journal of Natural Products 78: 1765-1796 (2015)
dx.doi.org/10.1021/np501065h
4. Reversibility of NP/RPA
280nm
230nm
A
K
0 0.125 0.25 0.375 0.5 0.625 0.75 0.875 1 1.14 1.33 1.6 2 2.67 4 8 ∞
IIII II
IIIII I1/K
GUESSmix in Hexane / Ethyl acetate / Methanol / Water 4:6:4:6
Reverse Phase
Normal Phase
G
H
X
T
r
C
D
F
R
U
V
A
Q
M
N
Z
E O
I
Y
b
6. High Speed Countercurrent
Chromatography (HSCCC)
§Minimal sample preparation
(direct chromatography of crude extracts)
§High mass – High resolution
§No sample loss (support-free
chromatography)
§Reproducibility
(scale-up or
scale down)
§Flexibility
8. elution method phase changea
flow
direction
change
rotation
direction
change
comments
classical – – – highly retained analytes remain in stationary
phase
EECCC single – – analytes elute in order of K values
BECCC – single – elution order reverses; some analytes may
elute at separate volumes
back-step CCC twice – – a plug of aqueous phase introduced to elute
highly retained analytes
dual-mode single single – elution order reverses
dual-rotation single single elution order reverses
multiple dual-mode multiple multiple – elution order reverses each cycle
ICcE multiple multiple – sample loop is in the middle of a single
column or between two separate columns
aphase change refers to switching mobile and stationary phase
Summary of Countercurrent Separation Elution Methods: Elution-extrusion
Countercurrent Chromatography (EECCC), Back-extrusion Countercurrent
Chromatography (BECCC), and Intermittent Countercurrent Extraction (ICcE)
CCS Methods
Friesen, J. B.; McAlpine, J. B.; Chen, S.-N.; Pauli, G. F., Countercurrent Separation of Natural Products: An Update. Journal
of Natural Products 2015, 78, 1765-1796.
9. Elution-extrusion CCC
Fig. 2. The elution extrusion method.
(A) The elution step; (B) starting the
extrusion step by switching the
entering fluid; (C) the extrusion step.
A solvent front
moves through the column. (D and E)
Close view of the circled area
showing the difference in velocities
between the solvent front, uM, and the
“stationary” phase velocity, uS. The
dotted area in (D) is squeezed to fill
the volume in (E).
Band broadening inside the chromatographic column: The interest of a
liquid stationary phase Journal of Chromatography A, Volume 1126,
Issues 1–2, 8 September 2006, Pages 347-356 Alain Berthod
11. Elution-Extrusion CCC
Berthod, A.*; Friesen, J. B.*; Inui, T.; Pauli, G. F. [*equal contribution]
Elution-Extrusion Countercurrent Chromatography: Theory and Concepts in Metabolic Analysis.
Anal. Chem. 2007, 79, 3371-3382.
12. B
i
DVi
VC
VC·VCM · VRi
-1
h
g
C
g h
A
injected samples (g-l)
g h
VM VS
VCM·KDi
-1
l k j i
D
ihg jk l
E
V0
VCM
VCM+VM
VCM+VR(h)
Stage I
classical
elution
Stage II
sweep
elution
Stage III
extrusion
SDMR VKVV ii
×+=
elution equation
i
i
D
CM
CCMEECCC
K
V
VVV -+=
extrusion equation
new SP
solvent front
new
SP
VM·VCM · VRi
-1
il k j
Equilibrium - Start of EECCC Run
End of EECCC Run
chromatogram volumes
VCM+VC
N = 1 2 3 4 5 6 7 8 9 10
calculation
MP
MP SP
MP
SP
new SP
SP
SP
SP
Berthod, A. Friesen, J.B. Inui, T. Pauli G.F. Analytical Chemistry 79, 3371-3382 (2007)
14. GUESSmix in HEMWat 4:6:4:6
0 0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.29 2.67 3.2 4 5.33 8 16 ¥K'(2)
A
0 0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.29 2.67 3.2 4 5.33 8 16 ¥K'(2)
A
280nm
230nm
J-type centrifuge 120 mL
Fast Centrifugal Partition Chromatography (FCPC) 200 mL
220 mg
440 mg
G
H
X
T
r
C
D
F
R
U
V
A
Q
M
N
Z
E O
I
Y
b
Instrument Comparison
15. HEMWat +3 VCM = 313 mL
0 0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.29 2.67 3.2 4 5.33 8 16 ∞
KD
A 280nm
230nm
I II III
r C
F
U
V
M
Q
N
Z E
O
b
HEMWat +3 VCM = 254.5 mL
0 0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.29 2.67 3.2 4 5.33 8 16 ∞KD
A
HEMWat +3 VCM = 228 mL
0 0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.29 2.67 3.2 4 5.33 8 16 ∞
KD
A
HEMWat +3 VCM = 162 mL
0 0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.29 2.67 3.2 4 5.33 8 16 ∞KD
A
I II III
I II III
I II III
a
b
c
d
MS
16. A
280nm
230nm
A
K
0 0.125 0.25 0.375 0.5 0.625 0.75 0.875 1 1.14 1.33 1.6 2 2.67 4 8 ∞
IIII II
IIIII I1/K
Reversed Phase
Normal Phase
G
H
X
T
r
C
D
F
R
U
V
A
Q
M
N
Z
E O
I
Y
b
17. KD
intervals
0
≤ KD < 0.0625
0.0625
≤ KD <
0.125
0.125
≤ KD < 0.25
0.25
≤ KD < 0.5
0.5
≤ KD <
1
1
≤ KD <
2
2
≤ KD <
4
4
≤ KD <
8
8
≤ KD <
16
16
≤ KD <
32
32
≤ KD <
∞
HEMWat
0 rXHTG DR CF
QUA
V
N ME Z O I Yb
DEMWat
0 rXHT G D C
FUV
A
RQ
ZMN
E
OI Yb
GUESS Mix in DEMWat 5:5:5:5
0 0.25 0.5 0.75 1 1.33 2 4 ∞K'(1)
A
HEMWat 0
0 0.25 0.5 0.75 1 1.33 2 4
∞K'(1)
A
280nm
230nm
O
I
Yb
Z
E
M
NA
VU
F
DRX
H
T
G
r
C
Q
I
X
H
T
r
G
D
C
F
U
V
A
R
Q
ZMNE
OIYb
18. EECCC applications
Fig. 2. “2VC” EECCC method for rapid screening of different HepEMWat liquid systems in reversed-phase separation mode.
CCC column of 140 mL. 3.0 mL/min, up to VCM (140 mL, 47 min, vertical dotted line) immediately followed by upper phase
flowing in the same direction; : 650 rpm: 20 mg crude extract dissolved in 2mL upper phase and 2mL lower phase.
Rapid and preparative separation of traditional Chinese medicine Evodia rutaecarpa employing elution-extrusion and back-extrusion counter-current chromatography: Comparative study
Journal of Chromatography A, Volume 1216, Issue 19, 8 May 2009, Pages 4140-4146 Yanbin Lu, Wenyan Ma, Ruilin Hu, Alain Berthod, Yuanjiang Pan
22. J Chromatogr A. 2012 Feb 3;1223:53-63. doi: 10.1016/j.chroma.2011.12.036. Overlapping elution-extrusion counter-current chromatography: a novel
method for efficient purification of natural cytotoxic andrographolides from Andrographis paniculata. Wu D, Cao X, Wu S.
Fig. 4. ethanol extracts of A. paniculata. (A) Standard elution–extrusion
CCC method (tCM = 140 m) repeated elution–extrusion in) and (BCCC
(tCM,1 = 140 min and tCM,2 = 415 min, tj,2 = 275 min); (C) the
overlapping elution–extrusion CCC (tCM,1 = 85 min and tCM,2 = 250
min, tj,2 = 165 min). Peak (1) corresponding to andrographolide (1) and
peak (2,3) corresponding 14-deoxy-andrographolide (2) and 14-deoxy-
11,12-didehydroandrographolide (3). Other conditions: injection mode:
injection before equilibrium; elution mode: head-to-tail; 2 mL/min;: 850
rpm; :30 ◦C; 234.3 mg; UV detection: 254 nm; VS = 160 mL and VM =
110 mL; HEMWat 5:5:4:6 was prepared using an on-demand
preparation mode,. (I), elution; (II), sweep elution; (III), extrusion. Red
arrow: the point to inject the sample and pump simultaneously mobile
phase. Blue arrow: the point to switch pumped solvent from mobile
phase to stationary phase. Red dashed arrow: without third injection of
sample. The white bar (below the each graph): the pumped solvent
phase is lower phase used as mobile phase. The blue bar: the pumped
solvent phase is upper phase used as stationary phase.
EECCC
applications
24. Fig. 2. Separation of the test mixture in different configurations. (a) EECCC in the reversed-phase mode; (b) EECCC in the normal-phase mode; (c) back extrusion in the
reversed-phase mode; and (d) back extrusion in the normal-phase mode. VCM = 224 mL. The colored bands correspond to the liquid phases collected at the CCC column outlet.
The X-axis shows the elution volume in mL and the corresponding KD distribution coefficient expressed as [conc. in organic phase]/[conc. in aq. phase]. Injected amounts in
2mL mobile phase:
1-catechol (12 mg); 2-benzoic acid (8 mg); 3-benzaldehyde (2 mg); 4-anisole (20 mg); and 5-cumene (17 mg).
Using the liquid nature of the stationary phase in counter-current chromatography: V. The back-extrusion method
Journal of Chromatography A, Volume 1189, Issues 1–2, 2 May 2008, Pages 10-18 Yanbin Lu, Yuanjiang Pan, Alain Berthod
Elution Methods: BECCC
25. Fig. 3. Fractionation of an ethanol extract of Piper longum L. (b) BECCC with VCM = 140 mL. (c) EECCC with VCM = 140 mL. (d) BECCC with VCM = 350 mL.
Liquid system: HEMWat 3/2/3/2, aqueous mobile phase: 2.9 mL/min; VC = 140 mL; rotor rotation: 650 rpm; VM =93mL; VS =47mL; Sf = 34%; UV detection:
254 nm. Sample injection: 50 mg of dry extract dissolved in 1mL upper organic phase + 1mL lower aqueous phase. See Fig. 2 legend.
Using the liquid nature of the stationary phase in counter-current chromatography: V. The back-extrusion method
Journal of Chromatography A, Volume 1189, Issues 1–2, 2 May 2008, Pages 10-18 Yanbin Lu, Yuanjiang Pan, Alain Berthod
Elution Methods: BECCC
34. Fig. 3. Diagram of the multiple dual mode set-up in the head-to-tail or descending position (A) and tail-to-head or
ascending position (B). Solute 1 elutes immediately in the descending step, and solutes 4 and 5 with a high affinity
for the upper phase elute in the second ascending step, while the remaining solutes 2 and 3 see increased separation
going back and forth in the following dual mode steps.
Purification of Coomassie Brilliant Blue G-250 by multiple dual mode countercurrent chromatography Journal of Chromatography A, Volume 1232, 6 April 2012, Pages 134-141
Nazim Mekaoui, Joseph Chamieh, Vincent Dugas, Claire Demesmay, Alain Berthod
Multiple Dual Mode
36. Fig. 7. Experimental separation of dinitrophenyl derivatives of serine (first peak) and aspartic acid (second peak). (A) Classical separation with a 130 mL hydrodynamic CCC column
and HEM/aqueous HCl 0.1 M; 4:5:4:5, lower aqueous mobile phase in the descending or head-to-tail direction at 0.35 mL/min, VS = 100 mL, VM = 30 mL, 800 rpm, detection UV
280 nm, KD1 = 0.77, KD2 = 0.90. (B) Classical separation but with mobile phase flow rate 2 mL/min, VS = 74 mL, VM = 56 mL; (C) MDM mode with 67 steps as indicated performed
with a constant flow rate of 2 mL/min for both liquid phases. (D) MDM mode with 33 steps of double volume and also constant flow of 2 mL/min.
Using the liquid nature of the stationary phase. VI. Theoretical study of multi-dual mode countercurrent chromatography Journal of Chromatography A,
Volume 1218, Issue 36, 9 September 2011, Pages 6061-6071 Nazim Mekaoui, Alain Berthod
Multiple Dual Mode
37. Fig. 4. Separation of polar and non-polar compounds
in Coomassie Blue G-250 (Acros #1) by dual-mode
elution and control by TLC. CCC conditions:
HepBuWat 2:3:4 system. 1000 rpm; both H → T
descending and T→ H ascending flow rates: 2
mL/min; Sf = 46%; injection volume: 1 mL (10 mg);
classical descending CM step for 38.5 min or 77 mL
aqueous phase (wavy blue band); dual mode DM step
until complete elution of the hydrophobic fraction at
78.5 min after 80 mL organic phase (dotted red band).
TLC conditions: silica gel on aluminum Plates 60
F254, 1-butanol/acetic acid/water 75:10:5 (v/v) eluting
phase. The TLC controlled fractions are indicated.
Purification of Coomassie Brilliant Blue G-250 by multiple dual mode countercurrent chromatography Journal of Chromatography A, Volume 1232, 6 April 2012, Pages 134-141
Nazim Mekaoui, Joseph Chamieh, Vincent Dugas, Claire Demesmay, Alain Berthod
Multiple Dual Mode
38. Fig. 5. 254 nm UV trace obtained during a “trapping” multi-dual-mode experiment for the purification of 500 mg of CBB G-250 (Acros #1).
Two coils serially connected (see Fig. 3 for experimental set-up). Total volume 140 mL. Rotor rotation: 1100 rpm; flow rate (both phases): 2
mL/min; Sf = 46%. Blue steps refer to head-to-tail descending elution step with the aqueous phase and orange to tail-to-head ascending step
with the organic upper phase. Repetitive 1 mL injections are indicated by arrows. The light yellow bands show the polar fraction elution (almost
colorless) collected in the aqueous phase. The pink bands shows the apolar blue fractions collected in the organic phase. The purified CBB
fraction was recovered in a long 70 mL head-to-tail aqueous phase elution after 155 min not shown due to complete detector saturation. See
Table 1 for full modeling of band locations inside the CCC columns.
Purification of Coomassie Brilliant Blue G-250 by multiple dual mode countercurrent chromatography Journal of Chromatography A, Volume 1232, 6 April 2012, Pages 134-141
Nazim Mekaoui, Joseph Chamieh, Vincent Dugas, Claire Demesmay, Alain Berthod
Multiple Dual Mode
43. Fig. 4. Chromatogram constructed from HPLC peak areas using an ICcE method
on a Midi-DE preparative column for the extraction of tritolide from a dried
down MPLC fraction from an ethanol extract of Tripterygium Wilfordii Hook. f.
(bioactive components – Triptolide (C1), K = 1.07; Peritassines A (C2), K = 2.90;
wilforigine (C3), K = 10.2 and wilforine (C4), K = 13.8); Solvent system:
HEMWat 15; upper phase flow rate 40ml/min; lower phase flow rate 35 ml/min;
flow switched every 4min; sample concentration: 12.0 g/l, sample volume:
766ml; rotational speed: 1250 rpm; upper phase detection wavelength: 226 nm;
lower phase detection wavelength: 220 nm; temperature: 30 ◦C.
188mg of triptolide at greater than
98% purity was separated from 9.2
g of crude extract, using 10 l of
solvent in
3h.
Intermittent counter-current extraction as an alternative approach to purification of Chinese herbal
medicine Journal of Chromatography A, Volume 1216, Issue 19, 8 May 2009, Pages 4187-4192 Peter
Hewitson, Svetlana Ignatova, Haoyu Ye, Lijuan Chen, Ian Sutherland
51. HSCCC chromatograms of the EPS with (A)OPB mode and (B) DPB mode. HSCCC conditions: solvent system: EBuWat (9:1:10); : 900
rpm; : 30 °C; flow rate: 1.8mL/min; detection wavelength: 280 nm; sample size: (A) 200mg of the EPS in 10 mL of the lower phase; (B)
50mg of the EPS in 5mL of the upper phase and 5mL of the lower phase.
In the HSCCC separation procedure, the two phases of the solvent
system EBuWat (9:1:10) were pumped into the coil column at a flow rate of
20 mL/min with two constant flow pumps. After the column was entirely
filled with the solvent system and rotating at 900 rpm, the flow rate of both
the two phases was adjusted to 2.2 mL/min. Only the lower phase was eluted
out from the column in the equilibration process. Equilibrium was established
when the two phases eluted from the outlet of the column had the same
volume
Phytochem Anal. 2015 Nov-Dec;26(6):444-53. doi: 10.1002/pca.2579. Rapid Separation of Three Proanthocyanidin Dimers from Iris lactea Pall.
var. Chinensis (Fisch.) Koidz by High-Speed Counter-Current Chromatography With Continuous Sample Load and Double-Pump Balancing Mode.
Lv H, Yuan Z, Wang X, Wang Z, Suo Y, Wang H.