SlideShare uma empresa Scribd logo
1 de 41
MOBILE PHASE
EFFECT OF PRESSURE
STATIONARY PHASE
PUMP
INJECTOR
OVEN
RESTRICTOR
COLUMN
DETECTOR
 MICRROPROCESOR
 Part of the theory of separation in SFC is based
on the density of supercritical fluid which
correspond to solvating power .As the pressure
in the system is increases, the supercritical
fluid density increases and correspondingly its
solvating power increases. Therefore as the
density of the supercritical fluid mobile phase
is increased , components retained in the
column can be made to elute. This is similar to
temperature programming in GC or using a
solvent gradient in HPLC.
 Density @ Solvating power
MOBILE PHASE/CARIIER=SUPERCRITICAL FLUID
SUPERCRITICAL FLUID=Any substance at a
temperature and pressure above its critical point ,
where distinct liquid & gas phase do not exist.
It can diffuse through solid like a gas and dissolve
material like liquid.
 Supercritical temperature= For every substance
there is temperature above which it can no longer
exist as a liquid, no matter how much pressure is
applied.
 Supercritical pressure= For every substance there
is a pressure above which the substance no longer
exist as gas , no matter how high the temperature
is raised.
 Supercritical fluid=A supercritical fluid is a
material that can be liquid or gas used in state
above critical temperature or critical pressure
where gas or liquid can co exist.
 LIQUID LIKE DENSITY INCREASED
 GAS LIKE VISCOSITY DECREASED
 GAS LIKE COMPRESIBILITY
 DIFFUSIBILITY ARE HIGHER THEN LIQUID
 REDUCTION IN SURFACE TENSION
 CO2 (MOST USED IN SFC)
 N2O (Nitrous oxide)
 Ethylene
 Propylene
 n-heptane
 Ethanol
 Propane
 Ammonia
 H2O
ADVANTAGE:
 LOW CRITICAL PRESSURE (74 atm )
 LOW CRITICAL TEMPERATURE ( 31c )
 CO2 is relatively non-toxic , non-flammable.
 High purity (available)
 Low cost
 Easily removable from extract
 CO2 IS LOW POLAR (LOW DIPOLE)
 CO2 + one or More co-solvent =increase polarity
 CAN NOT EXTRACT THE POLAR SOLUTES
NITROUS OXIDE (N2O)
ADV:
 GOOD FOR EXTRACTION OF POLAR
SOLUTES=B/C N2O HAS PERMANENT DIPOLE
MOMENT.
 EXAMPLE=N2O is better then CO2 for extraction
of Polychlorinates , Dibenzodioxines from flyash
(solid fuel produce during combustion )
 AT CRITICAL CONDITION IT CAN BE EXPLOSIVE.
H2O
DISADV:
 HIGH CRITICCAL PRESSURE ( 220 atm )
 HIGH CRITICAL TEMPERATURE (374c)
 AT THESE CONDITION H2O BECOMES CORROSIVE
(destroy solid material by chemical rxn ).
 THRESHOLD PRESSURE: A particular pressure at
which miscibility of solute & solvent is occur is
called threshold pressure.
 Pressure at which solute reaches its maximum
solubility.
 Knowledge of physical properties of solutes.
 Role=to modified the properties of solvent.
 Example= Alcohols, cyclic ethers, aceto-nitrile
and chloroform or ethyl acetate.
 The adding of modifier fluid improves the
solvating power of SF and sometimes enhances
selectivity of the separation.
 There are number of possible fluid which may be
used in SFC as the mobile phase .Mostly CO2 is
used.
 The main disadvantage of CO2 is its in ability to
elute very polar or ionic compounds.
 This can be overcome by adding a small portion of
a second fluid improves the solvating power of
the supercritical fluid and sometimes enhances
selectivity of the separation.
 Same as those for GC and LC, with some modification
 Silica/Alumina
 Useful for non-polar compounds
 Lead to irreversible adsorption of some
polar solutes
 Widely used polar stationary phase
 Poly-siloxanes :- stable, flexible Si…O bond lead to
good diffusion.
 Polymehtylsiloxanea: increase efficiency in
separating closely related polar analytes.
 Cyanopropyl polysiloxanes:- useful for compound
with COOH
 Pressure change in SFC is effect the retention time
and retention factor .The density of supercritical fluid
which correspond to solvating power .As the pressure
in the system is increases, the supercritical fluid
density increases and correspondingly its solvating
power increases. Which in turn to shorten the elution
time.
 Improvement in chromatogram realized by pressure
programming.
 In contact to HPLC Pumping system, Pressure
rather than flow control is necessary.
 In general, The type of High-pressure pump used
in SFC is determined by the column type=
I. For Packed column:- Reciprocating pumps are
generally used.(reciprocating pumps are allow
to easier mixing of the mobile phase or
introduction of modifier fluid.)
II. For capillary column:- Syringe pumps are
mostly employed.(Provide consistent pressure
for a neat mobile phase)
 The injector is required for sample inject into column.
 For Packed column:- A conventional HPLC
injection system is adequate.
 For Capillary column:- The sample volume
depend on column diameters.
The small sample volume must be quickly
injected into the column.
Therefore pneumatically driven valves are
required.
INJECTOR VOLUME
 Capillary column:- Injection volume >90nL
 Greater volume effect resolution.
 Packed column:- Injection volume >1uL
 A Thermostated column oven is required for precise
temperature control of the mobile.
 Convention GC & LC ovens are generally used.
RESTRICTOR=BACK PRESSURE
 It is used to maintain the desired pressure in the
column and to convert the eluent from
supercritical fluid to a gas for transfer to the
detector.
 It keeps mobile phase supercritical throughout
separation and often must be heated to prevent
clogging( block).
 One or more microprocessor are used in SFC
instrument to control pumping pressure, oven
temperature and detector performance.
 Once the sample is injected into the supercritical
stream it is carried into the analytical column.
The column contains a highly viscous liquid
(called a stationary phase) into which the analytes
can be temporarily adsorbed and then released
based on their chemical nature . This temporary
retention cause some analytes to remain longer in
the column and is what allow separation of the
mixture. Different types of stationary phase are
available with varying compositions and
polarities.
 There are two types column are used in SFC:
 Packed column & capillary column
 Both packed and open tubular columns are used.
Packed columns can provide more theoretical
plates and handle large volume than open tubular
columns.
 Packed column usually made up of
stainless steel,10 to 25cm.
 More than 1,00,000 plates have been achieved in
packed column.
 Open column :The column length is 10 to 20m. and
inside the diameter is 50 to 100mm common in open
tubular columns.
 For difficult separation column 60m (or) large have
been used.
 Typicallytheir are poly-siloxane chemically bounded
wall of capillary column.
 More analysis time.
 Less sample capacities.
 A major advantage of SFC over HPLC is that flame
ionization detector of gas can be employed .Mass
spectrometer are also more adapted as detector for SFC
then HPLC.
 Both HPLC and GC detector are compatible for
SFC.[UV,FID,FLOURESENCE DETECTOR]
 Choice depend on upon:
I. Mobile composition
II. Column type
III. Flow rate
Supercritical fluid chromatography| chromatographic techniques| by Gobind Kumar
Supercritical fluid chromatography| chromatographic techniques| by Gobind Kumar
Supercritical fluid chromatography| chromatographic techniques| by Gobind Kumar

Mais conteúdo relacionado

Mais procurados

Super critical fluid chromatography
Super critical fluid chromatographySuper critical fluid chromatography
Super critical fluid chromatographyceutics1315
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatographyabhisek Pradhan
 
Super critical fluid chromatography
Super critical fluid chromatographySuper critical fluid chromatography
Super critical fluid chromatographyDineshk117
 
VIVEK PINGALE - Copy
VIVEK PINGALE - CopyVIVEK PINGALE - Copy
VIVEK PINGALE - CopyVivek Pingale
 
Types of Distillation & column internals
Types of Distillation & column internalsTypes of Distillation & column internals
Types of Distillation & column internalsBharat Kumar
 
Flash distallation by khalid
Flash distallation by khalidFlash distallation by khalid
Flash distallation by khalidKhalid Nawaz
 
Fractional Distillation
Fractional DistillationFractional Distillation
Fractional DistillationUnnati Garg
 
Supercriticalfluidchromatography 140929003755-phpapp01
Supercriticalfluidchromatography 140929003755-phpapp01Supercriticalfluidchromatography 140929003755-phpapp01
Supercriticalfluidchromatography 140929003755-phpapp01Sai Datri Arige
 
Current advancement in different gas liquid operations
Current advancement in different gas liquid operationsCurrent advancement in different gas liquid operations
Current advancement in different gas liquid operationsSunny Chauhan
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatographyRituHaldive
 
Super critical fluid (SCF) for nanotechnology
Super critical fluid (SCF) for nanotechnologySuper critical fluid (SCF) for nanotechnology
Super critical fluid (SCF) for nanotechnologySarah Omran
 
Distillation
DistillationDistillation
DistillationAadil22
 

Mais procurados (20)

Super critical fluid chromatography
Super critical fluid chromatographySuper critical fluid chromatography
Super critical fluid chromatography
 
Saikanth(sfc)
Saikanth(sfc)Saikanth(sfc)
Saikanth(sfc)
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatography
 
Distillation.pdf
Distillation.pdfDistillation.pdf
Distillation.pdf
 
Super critical fluid chromatography
Super critical fluid chromatographySuper critical fluid chromatography
Super critical fluid chromatography
 
Continuous Distillation with Reflux Ratio
Continuous Distillation with Reflux RatioContinuous Distillation with Reflux Ratio
Continuous Distillation with Reflux Ratio
 
VIVEK PINGALE - Copy
VIVEK PINGALE - CopyVIVEK PINGALE - Copy
VIVEK PINGALE - Copy
 
Types of Distillation & column internals
Types of Distillation & column internalsTypes of Distillation & column internals
Types of Distillation & column internals
 
Flash distallation by khalid
Flash distallation by khalidFlash distallation by khalid
Flash distallation by khalid
 
Fractional Distillation
Fractional DistillationFractional Distillation
Fractional Distillation
 
Distillation
DistillationDistillation
Distillation
 
Supercriticalfluidchromatography 140929003755-phpapp01
Supercriticalfluidchromatography 140929003755-phpapp01Supercriticalfluidchromatography 140929003755-phpapp01
Supercriticalfluidchromatography 140929003755-phpapp01
 
Distillation
DistillationDistillation
Distillation
 
Current advancement in different gas liquid operations
Current advancement in different gas liquid operationsCurrent advancement in different gas liquid operations
Current advancement in different gas liquid operations
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatography
 
Gas absorption ppt
Gas absorption pptGas absorption ppt
Gas absorption ppt
 
Super critical fluid (SCF) for nanotechnology
Super critical fluid (SCF) for nanotechnologySuper critical fluid (SCF) for nanotechnology
Super critical fluid (SCF) for nanotechnology
 
Packed columns
Packed columnsPacked columns
Packed columns
 
distillation
distillationdistillation
distillation
 
Distillation
DistillationDistillation
Distillation
 

Semelhante a Supercritical fluid chromatography| chromatographic techniques| by Gobind Kumar

Supercritical Fluid Chromatography-lecture.pptx
Supercritical Fluid Chromatography-lecture.pptxSupercritical Fluid Chromatography-lecture.pptx
Supercritical Fluid Chromatography-lecture.pptxdevendergomi1998
 
Supercritical Fluid Chromatography
Supercritical Fluid ChromatographySupercritical Fluid Chromatography
Supercritical Fluid ChromatographyBHARATH_B
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatographyVARSHAAWASAR
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatographyVrushali Tambe
 
Supercritical Fluid Chromatography
Supercritical Fluid ChromatographySupercritical Fluid Chromatography
Supercritical Fluid ChromatographyDrBasavarajaiahSm
 
Supercritical fluid chromatography ppt practical
Supercritical fluid chromatography ppt practicalSupercritical fluid chromatography ppt practical
Supercritical fluid chromatography ppt practicalAMIT KANSE
 
Chapter 4 chromatography_b_2010
Chapter 4 chromatography_b_2010Chapter 4 chromatography_b_2010
Chapter 4 chromatography_b_2010drs_swylam
 
Pharmagupshup supercritical fluid chrometography and flash chromatography p...
Pharmagupshup supercritical fluid chrometography and flash chromatography   p...Pharmagupshup supercritical fluid chrometography and flash chromatography   p...
Pharmagupshup supercritical fluid chrometography and flash chromatography p...Hitesh Katariya
 
Supercritical chromatography
Supercritical chromatographySupercritical chromatography
Supercritical chromatographyGanesh Shinde
 
Instrumentation & App of SFC by Laiq
Instrumentation & App of SFC by LaiqInstrumentation & App of SFC by Laiq
Instrumentation & App of SFC by LaiqIMRANLAIQ1
 
Super Critical Fluid Chromatography
Super Critical Fluid ChromatographySuper Critical Fluid Chromatography
Super Critical Fluid ChromatographyPallavi Rushiya
 
SUPERCRITICAL FLUID EXTRACTION.pptx
SUPERCRITICAL FLUID EXTRACTION.pptxSUPERCRITICAL FLUID EXTRACTION.pptx
SUPERCRITICAL FLUID EXTRACTION.pptxSunaynaChoudhary
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatographySagar Savale
 
High Performance Liquid Chromatography..
High Performance Liquid Chromatography..High Performance Liquid Chromatography..
High Performance Liquid Chromatography..Somnath Patil
 

Semelhante a Supercritical fluid chromatography| chromatographic techniques| by Gobind Kumar (20)

Super critical FC
Super critical FCSuper critical FC
Super critical FC
 
Supercritical Fluid Chromatography-lecture.pptx
Supercritical Fluid Chromatography-lecture.pptxSupercritical Fluid Chromatography-lecture.pptx
Supercritical Fluid Chromatography-lecture.pptx
 
Supercritical Fluid Chromatography
Supercritical Fluid ChromatographySupercritical Fluid Chromatography
Supercritical Fluid Chromatography
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatography
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatography
 
Supercritical Fluid Chromatography
Supercritical Fluid ChromatographySupercritical Fluid Chromatography
Supercritical Fluid Chromatography
 
Supercritical fluid chromatography ppt practical
Supercritical fluid chromatography ppt practicalSupercritical fluid chromatography ppt practical
Supercritical fluid chromatography ppt practical
 
Super critical fluid
Super critical fluidSuper critical fluid
Super critical fluid
 
Chapter 4 chromatography_b_2010
Chapter 4 chromatography_b_2010Chapter 4 chromatography_b_2010
Chapter 4 chromatography_b_2010
 
HPLC
HPLCHPLC
HPLC
 
Pharmagupshup supercritical fluid chrometography and flash chromatography p...
Pharmagupshup supercritical fluid chrometography and flash chromatography   p...Pharmagupshup supercritical fluid chrometography and flash chromatography   p...
Pharmagupshup supercritical fluid chrometography and flash chromatography p...
 
Supercritical chromatography
Supercritical chromatographySupercritical chromatography
Supercritical chromatography
 
Instrumentation & App of SFC by Laiq
Instrumentation & App of SFC by LaiqInstrumentation & App of SFC by Laiq
Instrumentation & App of SFC by Laiq
 
Super Critical Fluid Chromatography
Super Critical Fluid ChromatographySuper Critical Fluid Chromatography
Super Critical Fluid Chromatography
 
HPLC
HPLC HPLC
HPLC
 
Super critical fluid chromatography
Super critical fluid chromatographySuper critical fluid chromatography
Super critical fluid chromatography
 
SUPERCRITICAL FLUID EXTRACTION.pptx
SUPERCRITICAL FLUID EXTRACTION.pptxSUPERCRITICAL FLUID EXTRACTION.pptx
SUPERCRITICAL FLUID EXTRACTION.pptx
 
Supercritical fluid chromatography
Supercritical fluid chromatographySupercritical fluid chromatography
Supercritical fluid chromatography
 
High Performance Liquid Chromatography..
High Performance Liquid Chromatography..High Performance Liquid Chromatography..
High Performance Liquid Chromatography..
 
HPLC.pptx
HPLC.pptxHPLC.pptx
HPLC.pptx
 

Último

Unit 3 Emotional Intelligence and Spiritual Intelligence.pdf
Unit 3 Emotional Intelligence and Spiritual Intelligence.pdfUnit 3 Emotional Intelligence and Spiritual Intelligence.pdf
Unit 3 Emotional Intelligence and Spiritual Intelligence.pdfDr Vijay Vishwakarma
 
The basics of sentences session 3pptx.pptx
The basics of sentences session 3pptx.pptxThe basics of sentences session 3pptx.pptx
The basics of sentences session 3pptx.pptxheathfieldcps1
 
Accessible Digital Futures project (20/03/2024)
Accessible Digital Futures project (20/03/2024)Accessible Digital Futures project (20/03/2024)
Accessible Digital Futures project (20/03/2024)Jisc
 
Basic Civil Engineering first year Notes- Chapter 4 Building.pptx
Basic Civil Engineering first year Notes- Chapter 4 Building.pptxBasic Civil Engineering first year Notes- Chapter 4 Building.pptx
Basic Civil Engineering first year Notes- Chapter 4 Building.pptxDenish Jangid
 
How to Manage Global Discount in Odoo 17 POS
How to Manage Global Discount in Odoo 17 POSHow to Manage Global Discount in Odoo 17 POS
How to Manage Global Discount in Odoo 17 POSCeline George
 
Plant propagation: Sexual and Asexual propapagation.pptx
Plant propagation: Sexual and Asexual propapagation.pptxPlant propagation: Sexual and Asexual propapagation.pptx
Plant propagation: Sexual and Asexual propapagation.pptxUmeshTimilsina1
 
Single or Multiple melodic lines structure
Single or Multiple melodic lines structureSingle or Multiple melodic lines structure
Single or Multiple melodic lines structuredhanjurrannsibayan2
 
Graduate Outcomes Presentation Slides - English
Graduate Outcomes Presentation Slides - EnglishGraduate Outcomes Presentation Slides - English
Graduate Outcomes Presentation Slides - Englishneillewis46
 
Application orientated numerical on hev.ppt
Application orientated numerical on hev.pptApplication orientated numerical on hev.ppt
Application orientated numerical on hev.pptRamjanShidvankar
 
Fostering Friendships - Enhancing Social Bonds in the Classroom
Fostering Friendships - Enhancing Social Bonds  in the ClassroomFostering Friendships - Enhancing Social Bonds  in the Classroom
Fostering Friendships - Enhancing Social Bonds in the ClassroomPooky Knightsmith
 
FSB Advising Checklist - Orientation 2024
FSB Advising Checklist - Orientation 2024FSB Advising Checklist - Orientation 2024
FSB Advising Checklist - Orientation 2024Elizabeth Walsh
 
Key note speaker Neum_Admir Softic_ENG.pdf
Key note speaker Neum_Admir Softic_ENG.pdfKey note speaker Neum_Admir Softic_ENG.pdf
Key note speaker Neum_Admir Softic_ENG.pdfAdmir Softic
 
80 ĐỀ THI THỬ TUYỂN SINH TIẾNG ANH VÀO 10 SỞ GD – ĐT THÀNH PHỐ HỒ CHÍ MINH NĂ...
80 ĐỀ THI THỬ TUYỂN SINH TIẾNG ANH VÀO 10 SỞ GD – ĐT THÀNH PHỐ HỒ CHÍ MINH NĂ...80 ĐỀ THI THỬ TUYỂN SINH TIẾNG ANH VÀO 10 SỞ GD – ĐT THÀNH PHỐ HỒ CHÍ MINH NĂ...
80 ĐỀ THI THỬ TUYỂN SINH TIẾNG ANH VÀO 10 SỞ GD – ĐT THÀNH PHỐ HỒ CHÍ MINH NĂ...Nguyen Thanh Tu Collection
 
Understanding Accommodations and Modifications
Understanding  Accommodations and ModificationsUnderstanding  Accommodations and Modifications
Understanding Accommodations and ModificationsMJDuyan
 
Beyond_Borders_Understanding_Anime_and_Manga_Fandom_A_Comprehensive_Audience_...
Beyond_Borders_Understanding_Anime_and_Manga_Fandom_A_Comprehensive_Audience_...Beyond_Borders_Understanding_Anime_and_Manga_Fandom_A_Comprehensive_Audience_...
Beyond_Borders_Understanding_Anime_and_Manga_Fandom_A_Comprehensive_Audience_...Pooja Bhuva
 
Towards a code of practice for AI in AT.pptx
Towards a code of practice for AI in AT.pptxTowards a code of practice for AI in AT.pptx
Towards a code of practice for AI in AT.pptxJisc
 
UGC NET Paper 1 Mathematical Reasoning & Aptitude.pdf
UGC NET Paper 1 Mathematical Reasoning & Aptitude.pdfUGC NET Paper 1 Mathematical Reasoning & Aptitude.pdf
UGC NET Paper 1 Mathematical Reasoning & Aptitude.pdfNirmal Dwivedi
 
Holdier Curriculum Vitae (April 2024).pdf
Holdier Curriculum Vitae (April 2024).pdfHoldier Curriculum Vitae (April 2024).pdf
Holdier Curriculum Vitae (April 2024).pdfagholdier
 
Kodo Millet PPT made by Ghanshyam bairwa college of Agriculture kumher bhara...
Kodo Millet  PPT made by Ghanshyam bairwa college of Agriculture kumher bhara...Kodo Millet  PPT made by Ghanshyam bairwa college of Agriculture kumher bhara...
Kodo Millet PPT made by Ghanshyam bairwa college of Agriculture kumher bhara...pradhanghanshyam7136
 
How to setup Pycharm environment for Odoo 17.pptx
How to setup Pycharm environment for Odoo 17.pptxHow to setup Pycharm environment for Odoo 17.pptx
How to setup Pycharm environment for Odoo 17.pptxCeline George
 

Último (20)

Unit 3 Emotional Intelligence and Spiritual Intelligence.pdf
Unit 3 Emotional Intelligence and Spiritual Intelligence.pdfUnit 3 Emotional Intelligence and Spiritual Intelligence.pdf
Unit 3 Emotional Intelligence and Spiritual Intelligence.pdf
 
The basics of sentences session 3pptx.pptx
The basics of sentences session 3pptx.pptxThe basics of sentences session 3pptx.pptx
The basics of sentences session 3pptx.pptx
 
Accessible Digital Futures project (20/03/2024)
Accessible Digital Futures project (20/03/2024)Accessible Digital Futures project (20/03/2024)
Accessible Digital Futures project (20/03/2024)
 
Basic Civil Engineering first year Notes- Chapter 4 Building.pptx
Basic Civil Engineering first year Notes- Chapter 4 Building.pptxBasic Civil Engineering first year Notes- Chapter 4 Building.pptx
Basic Civil Engineering first year Notes- Chapter 4 Building.pptx
 
How to Manage Global Discount in Odoo 17 POS
How to Manage Global Discount in Odoo 17 POSHow to Manage Global Discount in Odoo 17 POS
How to Manage Global Discount in Odoo 17 POS
 
Plant propagation: Sexual and Asexual propapagation.pptx
Plant propagation: Sexual and Asexual propapagation.pptxPlant propagation: Sexual and Asexual propapagation.pptx
Plant propagation: Sexual and Asexual propapagation.pptx
 
Single or Multiple melodic lines structure
Single or Multiple melodic lines structureSingle or Multiple melodic lines structure
Single or Multiple melodic lines structure
 
Graduate Outcomes Presentation Slides - English
Graduate Outcomes Presentation Slides - EnglishGraduate Outcomes Presentation Slides - English
Graduate Outcomes Presentation Slides - English
 
Application orientated numerical on hev.ppt
Application orientated numerical on hev.pptApplication orientated numerical on hev.ppt
Application orientated numerical on hev.ppt
 
Fostering Friendships - Enhancing Social Bonds in the Classroom
Fostering Friendships - Enhancing Social Bonds  in the ClassroomFostering Friendships - Enhancing Social Bonds  in the Classroom
Fostering Friendships - Enhancing Social Bonds in the Classroom
 
FSB Advising Checklist - Orientation 2024
FSB Advising Checklist - Orientation 2024FSB Advising Checklist - Orientation 2024
FSB Advising Checklist - Orientation 2024
 
Key note speaker Neum_Admir Softic_ENG.pdf
Key note speaker Neum_Admir Softic_ENG.pdfKey note speaker Neum_Admir Softic_ENG.pdf
Key note speaker Neum_Admir Softic_ENG.pdf
 
80 ĐỀ THI THỬ TUYỂN SINH TIẾNG ANH VÀO 10 SỞ GD – ĐT THÀNH PHỐ HỒ CHÍ MINH NĂ...
80 ĐỀ THI THỬ TUYỂN SINH TIẾNG ANH VÀO 10 SỞ GD – ĐT THÀNH PHỐ HỒ CHÍ MINH NĂ...80 ĐỀ THI THỬ TUYỂN SINH TIẾNG ANH VÀO 10 SỞ GD – ĐT THÀNH PHỐ HỒ CHÍ MINH NĂ...
80 ĐỀ THI THỬ TUYỂN SINH TIẾNG ANH VÀO 10 SỞ GD – ĐT THÀNH PHỐ HỒ CHÍ MINH NĂ...
 
Understanding Accommodations and Modifications
Understanding  Accommodations and ModificationsUnderstanding  Accommodations and Modifications
Understanding Accommodations and Modifications
 
Beyond_Borders_Understanding_Anime_and_Manga_Fandom_A_Comprehensive_Audience_...
Beyond_Borders_Understanding_Anime_and_Manga_Fandom_A_Comprehensive_Audience_...Beyond_Borders_Understanding_Anime_and_Manga_Fandom_A_Comprehensive_Audience_...
Beyond_Borders_Understanding_Anime_and_Manga_Fandom_A_Comprehensive_Audience_...
 
Towards a code of practice for AI in AT.pptx
Towards a code of practice for AI in AT.pptxTowards a code of practice for AI in AT.pptx
Towards a code of practice for AI in AT.pptx
 
UGC NET Paper 1 Mathematical Reasoning & Aptitude.pdf
UGC NET Paper 1 Mathematical Reasoning & Aptitude.pdfUGC NET Paper 1 Mathematical Reasoning & Aptitude.pdf
UGC NET Paper 1 Mathematical Reasoning & Aptitude.pdf
 
Holdier Curriculum Vitae (April 2024).pdf
Holdier Curriculum Vitae (April 2024).pdfHoldier Curriculum Vitae (April 2024).pdf
Holdier Curriculum Vitae (April 2024).pdf
 
Kodo Millet PPT made by Ghanshyam bairwa college of Agriculture kumher bhara...
Kodo Millet  PPT made by Ghanshyam bairwa college of Agriculture kumher bhara...Kodo Millet  PPT made by Ghanshyam bairwa college of Agriculture kumher bhara...
Kodo Millet PPT made by Ghanshyam bairwa college of Agriculture kumher bhara...
 
How to setup Pycharm environment for Odoo 17.pptx
How to setup Pycharm environment for Odoo 17.pptxHow to setup Pycharm environment for Odoo 17.pptx
How to setup Pycharm environment for Odoo 17.pptx
 

Supercritical fluid chromatography| chromatographic techniques| by Gobind Kumar

  • 1.
  • 2. MOBILE PHASE EFFECT OF PRESSURE STATIONARY PHASE PUMP INJECTOR OVEN RESTRICTOR COLUMN DETECTOR  MICRROPROCESOR
  • 3.
  • 4.  Part of the theory of separation in SFC is based on the density of supercritical fluid which correspond to solvating power .As the pressure in the system is increases, the supercritical fluid density increases and correspondingly its solvating power increases. Therefore as the density of the supercritical fluid mobile phase is increased , components retained in the column can be made to elute. This is similar to temperature programming in GC or using a solvent gradient in HPLC.  Density @ Solvating power
  • 5.
  • 6.
  • 7. MOBILE PHASE/CARIIER=SUPERCRITICAL FLUID SUPERCRITICAL FLUID=Any substance at a temperature and pressure above its critical point , where distinct liquid & gas phase do not exist. It can diffuse through solid like a gas and dissolve material like liquid.
  • 8.  Supercritical temperature= For every substance there is temperature above which it can no longer exist as a liquid, no matter how much pressure is applied.  Supercritical pressure= For every substance there is a pressure above which the substance no longer exist as gas , no matter how high the temperature is raised.  Supercritical fluid=A supercritical fluid is a material that can be liquid or gas used in state above critical temperature or critical pressure where gas or liquid can co exist.
  • 9.  LIQUID LIKE DENSITY INCREASED  GAS LIKE VISCOSITY DECREASED  GAS LIKE COMPRESIBILITY  DIFFUSIBILITY ARE HIGHER THEN LIQUID  REDUCTION IN SURFACE TENSION
  • 10.
  • 11.  CO2 (MOST USED IN SFC)  N2O (Nitrous oxide)  Ethylene  Propylene  n-heptane  Ethanol  Propane  Ammonia  H2O
  • 12.
  • 13. ADVANTAGE:  LOW CRITICAL PRESSURE (74 atm )  LOW CRITICAL TEMPERATURE ( 31c )  CO2 is relatively non-toxic , non-flammable.  High purity (available)  Low cost  Easily removable from extract  CO2 IS LOW POLAR (LOW DIPOLE)  CO2 + one or More co-solvent =increase polarity
  • 14.  CAN NOT EXTRACT THE POLAR SOLUTES NITROUS OXIDE (N2O) ADV:  GOOD FOR EXTRACTION OF POLAR SOLUTES=B/C N2O HAS PERMANENT DIPOLE MOMENT.  EXAMPLE=N2O is better then CO2 for extraction of Polychlorinates , Dibenzodioxines from flyash (solid fuel produce during combustion )
  • 15.  AT CRITICAL CONDITION IT CAN BE EXPLOSIVE. H2O DISADV:  HIGH CRITICCAL PRESSURE ( 220 atm )  HIGH CRITICAL TEMPERATURE (374c)  AT THESE CONDITION H2O BECOMES CORROSIVE (destroy solid material by chemical rxn ).
  • 16.  THRESHOLD PRESSURE: A particular pressure at which miscibility of solute & solvent is occur is called threshold pressure.  Pressure at which solute reaches its maximum solubility.  Knowledge of physical properties of solutes.
  • 17.  Role=to modified the properties of solvent.  Example= Alcohols, cyclic ethers, aceto-nitrile and chloroform or ethyl acetate.  The adding of modifier fluid improves the solvating power of SF and sometimes enhances selectivity of the separation.
  • 18.  There are number of possible fluid which may be used in SFC as the mobile phase .Mostly CO2 is used.  The main disadvantage of CO2 is its in ability to elute very polar or ionic compounds.  This can be overcome by adding a small portion of a second fluid improves the solvating power of the supercritical fluid and sometimes enhances selectivity of the separation.
  • 19.  Same as those for GC and LC, with some modification  Silica/Alumina  Useful for non-polar compounds  Lead to irreversible adsorption of some polar solutes  Widely used polar stationary phase  Poly-siloxanes :- stable, flexible Si…O bond lead to good diffusion.  Polymehtylsiloxanea: increase efficiency in separating closely related polar analytes.  Cyanopropyl polysiloxanes:- useful for compound with COOH
  • 20.  Pressure change in SFC is effect the retention time and retention factor .The density of supercritical fluid which correspond to solvating power .As the pressure in the system is increases, the supercritical fluid density increases and correspondingly its solvating power increases. Which in turn to shorten the elution time.  Improvement in chromatogram realized by pressure programming.
  • 21.
  • 22.
  • 23.  In contact to HPLC Pumping system, Pressure rather than flow control is necessary.  In general, The type of High-pressure pump used in SFC is determined by the column type= I. For Packed column:- Reciprocating pumps are generally used.(reciprocating pumps are allow to easier mixing of the mobile phase or introduction of modifier fluid.) II. For capillary column:- Syringe pumps are mostly employed.(Provide consistent pressure for a neat mobile phase)
  • 24.
  • 25.
  • 26.
  • 27.
  • 28.
  • 29.
  • 30.  The injector is required for sample inject into column.  For Packed column:- A conventional HPLC injection system is adequate.  For Capillary column:- The sample volume depend on column diameters. The small sample volume must be quickly injected into the column. Therefore pneumatically driven valves are required. INJECTOR VOLUME  Capillary column:- Injection volume >90nL  Greater volume effect resolution.  Packed column:- Injection volume >1uL
  • 31.
  • 32.  A Thermostated column oven is required for precise temperature control of the mobile.  Convention GC & LC ovens are generally used.
  • 33. RESTRICTOR=BACK PRESSURE  It is used to maintain the desired pressure in the column and to convert the eluent from supercritical fluid to a gas for transfer to the detector.  It keeps mobile phase supercritical throughout separation and often must be heated to prevent clogging( block).
  • 34.  One or more microprocessor are used in SFC instrument to control pumping pressure, oven temperature and detector performance.
  • 35.  Once the sample is injected into the supercritical stream it is carried into the analytical column. The column contains a highly viscous liquid (called a stationary phase) into which the analytes can be temporarily adsorbed and then released based on their chemical nature . This temporary retention cause some analytes to remain longer in the column and is what allow separation of the mixture. Different types of stationary phase are available with varying compositions and polarities.  There are two types column are used in SFC:  Packed column & capillary column
  • 36.  Both packed and open tubular columns are used. Packed columns can provide more theoretical plates and handle large volume than open tubular columns.  Packed column usually made up of stainless steel,10 to 25cm.  More than 1,00,000 plates have been achieved in packed column.
  • 37.  Open column :The column length is 10 to 20m. and inside the diameter is 50 to 100mm common in open tubular columns.  For difficult separation column 60m (or) large have been used.  Typicallytheir are poly-siloxane chemically bounded wall of capillary column.  More analysis time.  Less sample capacities.
  • 38.  A major advantage of SFC over HPLC is that flame ionization detector of gas can be employed .Mass spectrometer are also more adapted as detector for SFC then HPLC.  Both HPLC and GC detector are compatible for SFC.[UV,FID,FLOURESENCE DETECTOR]  Choice depend on upon: I. Mobile composition II. Column type III. Flow rate