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Effect of temperature programming and compound chemistry
in Gas Chromatography
NAME: MOLOY ROY
COURSE: M.PHARM(1ST YEAR)
ROLL NO:2214063
PHARMACEUTICAL ANALYSIS
DR.B.C ROY COLLEGE OF PHARMACY AND ALLIED HEALTH SCIENCE, DURGAPUR, WESTBENGAL
1
CONTENT
1. What is Gas Chromatography(GC)?
2. Instrumentation of GC and relevant problem arise with the constant temperature :
3. What is temperature programming in Gas Chromatography?? And why it is needed..
4. Graphical representation of PTGC
5. Reference
2
TOPIC SLIDE NUMBER
3-3
4-4
5-5
6-6
8-8
What is Gas Chromatography(GC)?
• Separation techniques used as analytical purpose in pharmaceutical industries.
• Used for the separation of volatiles substances and can easily transformed in to gaseous form
• Two types –(based on stationary phase)
1. Gas-liquid (GLC) stationary phase – liquid, mobile phase-gas.
2. Gas -solid (GSC) stationary phase- solid, mobile phase- gas
Principle
ADSORPTION
PARTITION
BASED ON INTERMOLECULAR FORCES
BETWEEN adsorbate (sample to be analyzed)
AND adsorbent(stationary phase)
Ex: chlorophyll and xanthophyll separation is the
first experiment of chromatography
A SOLUTE WILL DISTRIBUTE ITSELF
BETWEEN TWO IMMISCIBLE LIQUIDS
ACCORDING TO ITS PARTITION
COEFFICIENT.
Ex: lower fatty acid experiment was the first GC
experiment
3
Instrumentation of GC and Relevant problem arise with constant temperature :
Image Source: Bitesize Bio https://microbenotes.com/gas-chromatography/
Column thermostatically controlled oven
(Mobile phase)
Liquid/gas
(in gaseous
phase
Incase of constant temperature
problems are :-
• HIGHER TEMP: Poor resolution /
Peaks are closely space (earlier
elution )
• LOWER TEMP:
Peaks are broad ,widely
spaced,excessive resolution
Compound having high-boiling point
are undetected due to immobility/ or
stickiness to stationary phase .(late
elution)
4
Low boiling point compound or small
sized particle eluted first and then
highly boiling point or respectively
larger sized particle compound was
eluted
What is temperature programming in Gas Chromatography?? And
why it temperature programming needed
• Temperature programming is the series of changing of temperature in column through out the
analysis. It maintain the temperature through out the process of analysis.
• The programmed temperature process commonly consists of an initial isothermal period then
liner temperature rise segment, then final isothermal period. But temperature programming
may varies according to our need – high resolution of peak (slow rate ) or cut down the
analysis time (rapid change).
• In temperature programming, those effects are overcome by maintaining a low temperature for
a short period of time, and increasing the temperature to help force out the longer-‘sticking’
compounds. This changes the retention time compared to a isothermal run.
5
Temperature programming is
basically necessary to get the
better result along with the
specific time of analysis
EXAMPLE OF PTGC- SEPERATION OF CAFFEINE
6
http://svmsl.chem.cmu.edu/vmsl/Caffeine/caffeine_temperature.htm
Graphical represention of PTGC
7
30ºC/Min ; 40ºC
5ºC/Min ; 40ºC
75ºC ;
CONSTANT
TEMPERATURE
8
R E F E R E N C E
1. https://chem.libretexts.org/Courses/BethuneCookman_University/B-CU%3A_CH-
345_Quantitative_Analysis/Book%3A_Analytical_Chemistry_2.1_(Harvey)/12%3A_Chromatographic_and_Electrophoretic_
Methods/12.04%3A_Gas_Chromatography (accessed on 06/11/2022 11:19 am)
2. http://svmsl.chem.cmu.edu/vmsl/Caffeine/caffeine_temperature.htm (accessed on 05/11/2022 08:20pm)
3. VOGEL’S TEXT BOOK OF QUANTITATIVE CHEMICAL ANALYSIS, 6TH EDITION; CHAPTER 9; 272-291

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Effect of temperature programming and compound chemistry in.pptx

  • 1. Effect of temperature programming and compound chemistry in Gas Chromatography NAME: MOLOY ROY COURSE: M.PHARM(1ST YEAR) ROLL NO:2214063 PHARMACEUTICAL ANALYSIS DR.B.C ROY COLLEGE OF PHARMACY AND ALLIED HEALTH SCIENCE, DURGAPUR, WESTBENGAL 1
  • 2. CONTENT 1. What is Gas Chromatography(GC)? 2. Instrumentation of GC and relevant problem arise with the constant temperature : 3. What is temperature programming in Gas Chromatography?? And why it is needed.. 4. Graphical representation of PTGC 5. Reference 2 TOPIC SLIDE NUMBER 3-3 4-4 5-5 6-6 8-8
  • 3. What is Gas Chromatography(GC)? • Separation techniques used as analytical purpose in pharmaceutical industries. • Used for the separation of volatiles substances and can easily transformed in to gaseous form • Two types –(based on stationary phase) 1. Gas-liquid (GLC) stationary phase – liquid, mobile phase-gas. 2. Gas -solid (GSC) stationary phase- solid, mobile phase- gas Principle ADSORPTION PARTITION BASED ON INTERMOLECULAR FORCES BETWEEN adsorbate (sample to be analyzed) AND adsorbent(stationary phase) Ex: chlorophyll and xanthophyll separation is the first experiment of chromatography A SOLUTE WILL DISTRIBUTE ITSELF BETWEEN TWO IMMISCIBLE LIQUIDS ACCORDING TO ITS PARTITION COEFFICIENT. Ex: lower fatty acid experiment was the first GC experiment 3
  • 4. Instrumentation of GC and Relevant problem arise with constant temperature : Image Source: Bitesize Bio https://microbenotes.com/gas-chromatography/ Column thermostatically controlled oven (Mobile phase) Liquid/gas (in gaseous phase Incase of constant temperature problems are :- • HIGHER TEMP: Poor resolution / Peaks are closely space (earlier elution ) • LOWER TEMP: Peaks are broad ,widely spaced,excessive resolution Compound having high-boiling point are undetected due to immobility/ or stickiness to stationary phase .(late elution) 4 Low boiling point compound or small sized particle eluted first and then highly boiling point or respectively larger sized particle compound was eluted
  • 5. What is temperature programming in Gas Chromatography?? And why it temperature programming needed • Temperature programming is the series of changing of temperature in column through out the analysis. It maintain the temperature through out the process of analysis. • The programmed temperature process commonly consists of an initial isothermal period then liner temperature rise segment, then final isothermal period. But temperature programming may varies according to our need – high resolution of peak (slow rate ) or cut down the analysis time (rapid change). • In temperature programming, those effects are overcome by maintaining a low temperature for a short period of time, and increasing the temperature to help force out the longer-‘sticking’ compounds. This changes the retention time compared to a isothermal run. 5 Temperature programming is basically necessary to get the better result along with the specific time of analysis
  • 6. EXAMPLE OF PTGC- SEPERATION OF CAFFEINE 6 http://svmsl.chem.cmu.edu/vmsl/Caffeine/caffeine_temperature.htm
  • 7. Graphical represention of PTGC 7 30ºC/Min ; 40ºC 5ºC/Min ; 40ºC 75ºC ; CONSTANT TEMPERATURE
  • 8. 8 R E F E R E N C E 1. https://chem.libretexts.org/Courses/BethuneCookman_University/B-CU%3A_CH- 345_Quantitative_Analysis/Book%3A_Analytical_Chemistry_2.1_(Harvey)/12%3A_Chromatographic_and_Electrophoretic_ Methods/12.04%3A_Gas_Chromatography (accessed on 06/11/2022 11:19 am) 2. http://svmsl.chem.cmu.edu/vmsl/Caffeine/caffeine_temperature.htm (accessed on 05/11/2022 08:20pm) 3. VOGEL’S TEXT BOOK OF QUANTITATIVE CHEMICAL ANALYSIS, 6TH EDITION; CHAPTER 9; 272-291