PFT902 - Gas Chromatography in Pharmaceutical Analysis

Outline info
Semester
School
Last revision date 2017-05-29 00:41:38.934
Last review date 2017-07-17 00:16:30.921


Subject Title
Gas Chromatography in Pharmaceutical Analysis

Subject Description
Gas Chromatography is the most widely used analytical technique for the separation and analysis of organic compounds. The efficiency of capillary columns, the sensitivity and selectivity of the detectors and the fully automated GC systems available make Gas Chromatography indispensable for any analytical laboratory. (Lectures and Labs)

Credit Status
One credit towards the Pharmaceutical Instrumentation Analyst (PIA) Certificate Program

Learning Outcomes
Upon successful completion of this subject the student will be able to:

1. Demonstrate a basic understanding of the advanced principles and practice of Gas Chromatography and understand how individual elements interrelate.

2. Competently use analytical methods on a gas chromatograph to produce valid analytical data.

3. Demonstrate a detailed comprehension of the following: GC requirements, GC separation parameters, packed and capillary columns, GC operation, GC detectors operation, GC troubleshooting techniques, basics of method validation and quantitative analysis.

4. Demonstrate solid knowledge of GC operation, maintenance and troubleshooting.

5. Comply with the basic good laboratory practice rules for accurate, reliable and get it right-first analysis.

6. Change and install GC parts as inject system and columns.

7. Competently set up the basic GC conditions to develop a GC method based on the chemical structure and properties of the components to be separated.

8. Operate independently a GC instrument using ChemStation software.

9. Set up, run and reprocess complex sequences consisting of standard injections, system suitability injections and multiples sample injections using ChemStation software.

Cheating and Plagiarism
Each student should be aware of the College's policy regarding Cheating and Plagiarism. Seneca's Academic Policy will be strictly enforced.

To support academic honesty at Seneca College, all work submitted by students may be reviewed for authenticity and originality, utilizing software tools and third party services. Please visit the Academic Honesty site on http://library.senecacollege.ca for further information regarding cheating and plagiarism policies and procedures.

Discrimination/Harassment
All students and employees have the right to study and work in an environment that is free from discrimination and/or harassment. Language or activities that defeat this objective violate the College Policy on Discrimination/Harassment and shall not be tolerated. Information and assistance are available from the Student Conduct Office at student.conduct@senecacollege.ca.

Accommodation for Students with Disabilities
The College will provide reasonable accommodation to students with disabilities in order to promote academic success. If you require accommodation, contact the Counselling and Disabilities Services Office at ext. 22900 to initiate the process for documenting, assessing and implementing your individual accommodation needs.

Prerequisite(s)
None

Topic Outline
7 WEEK MODE

General Theory of Gas Chromatography

  • WHMIS overview
  • Principle of separation
  • Basic concepts and terms
  • Instrumentation overview
  • Inlet systems for gas chromatography
  • Lab Experiment #1: Basic operation of ChemStation software

Columns in Gas Chromatography
  • Supports and adsorbents
  • Stationary phases
  • Column evaluation
  • Conditioning, column care and column installation
  • Packed columns
  • Capillary columns
  • Lab Experiment #2: GC separation of Chlorinated Solvents using packed column and isothermal method

Gas Chromatography Detectors
  • General aspects (noise, sensitivity, selectivity, limit of detection, response factor, practical considerations)
  • Thermal Conductivity Detector (TCD)
  • Flame Ionization Detector (ECD)
  • Introduction to Mass Spectrometer Detector 9GC-MS)
  • Lab Experiment #3: GC separation of Polynuclear Aromatic Hydrocarbons using packed column and TPGC
  • Assignment #1

Optimization of Separation Conditions
  • Basic choices
  • Packed versus capillary columns
  • The influences of column variables (inner diameter, length)
  • The influences of operational variables (carrier-gas velocity, column temperature, isothermal separation, temperature programmed operation)
  • Lab Experiment  #4: GC separation of Aromatic and Aliphatic Solvents using capillary column and split injection
  • Quiz

Qualitative and Quantitative Analysis by GC
  • Statistics of quantitative calculations
  • Errors to be avoided in making measurements
  • Methods of quantitative analysis (area normalization, area normalization with response factor, external standard and internal standard method)
  • Qualitative analysis (retention parameters)
  • Lab Experiment #5: GC separation of Alcohol Solvents using capillary column and split injection
  • Assignment #2

Basics of Method Validation and Troubleshooting in GC
  • Definition and description of method validation parameters (system suitability, specificity, limit of detection (LOD), limit of quantitation (LOQ), linearity, accuracy, precision, intermediate precision, robustness
  • Chromatographic interpretation of different peak shapes encountered in gas chromatography (assign possible cause to the symptom)
  • Lab Experiment #6: GC separation of Residual Solvents using capillary column and Head Space unit injection

14 WEEK MODE

General Theory of Gas Chromatography
  • WHMIS overview
  • Principle of separation
  • Basic concepts and terms
  • Instrumentation overview
  • Inlet systems for gas chromatography

Columns in Gas Chromatography
  • Supports and adsorbents
  • Stationary phases
  • Column evaluation
  • Conditioning, column care and column installation
  • Packed columns
  • Capillary columns

Gas Chromatography Detectors
  • General aspects (noise, sensitivity, selectivity, limit of detection, response factor, practical consideration)
  • Thermal Conductivity Detector (TCD)
  • Flame Ionization Detector (FID)
  • Electron Capture Detector (ECD)
  • Introduction to Mass Spectrometer Detector (GC-MS)

Lab Experiment #1: Basic operation of ChemStation Software

Lab Experiment #2: GC separation of Chlorinated Solvents using packed columns, and isothermal method.

Optimization of Separation Conditions
  • Basic choices
  • Packed versus capillary columns
  • The influences of column variables (inner diameter, length)
  • The influences of operational variables (carrier-gas velocity, column temperature, isothermal separation, temperature programmed operation)

Qualitative and Quantitative Analysis by GC
  • Statistics of quantitative calculations
  • Errors to be avoided in making measurements
  • Methods of quantitative analysis (area normalization, area normalization with response factor, external standard and internal standard method)
  • Quiz

Lab Experiment #3: GC separation of Polynuclear Aromatic Hydrocarbons using packed column and TPGC method
Assignment # 1

Lab Experiment #4: GC separation of Aromatic and Aliphatic Solvents using capillary column and split injection

Lab Experiment #5: GC separation of Alcohol Solvents using capillary column and split injection
Assignment #2

Troubleshooting in GC
  • Chromatographic interpretation of different peak shapes encountered in gas chromatography (assign possible cause to the symptom)

Lab Experiment # 6: GC separation of Residual Solvents using capillary column and Head Space unit injection

Basics of Method Validation
  • Definition and description of method validation parameters (system suitability, specificity, limit of detection (LOD), limit of Quantitation (LOQ), linearity, accuracy, precision, intermediate precision, robustness)

Mode of Instruction
Lecture, labs, interactive quizzes and case studies

Prescribed Texts
None

Reference Material
Modern Practice of Gas Chromatography, Fourth Edition, R.L Grob, E.F. Barry, J. Wiley & Sons Inc. Publication, 2004 ISBN: 978-0471229834

Required Supplies
None

Promotion Policy

Grading Policy
A+ 90%  to  100%
A 80%  to  89%
B+ 75%  to  79%
B 70%  to  74%
C+ 65%  to  69%
C 60%  to  64%
D+ 55%  to  59%
D 50%  to  54%
F 0%    to  49% (Not a Pass)
OR
EXC Excellent
SAT Satisfactory
UNSAT Unsatisfactory

For further information, see a copy of the Academic Policy, available online (http://www.senecacollege.ca/academic-policy) or at Seneca's Registrar's Offices.


Modes of Evaluation
Assignments

  • Assignments are due at the beginning of the class on which they are due.
  • A late penalty of 10% per day is assessed for late assignments, including those not handed in at the beginning of class when due.
  • Material will not be accepted after one week following the due date and/or when the marked material is returned to students, whichever comes first.
  • Assignments are to be prepared by computer.

Absenteeism and Exams
  • Students should be aware that absenteeism almost guarantees an inability to achieve satisfactory grades.
  • Students who are absent for an examination due to an emergency (e.g., motor vehicle accident, hospitalization or death in the family) may provide official documentation within five days of the missed exam and be provided a deferred exam at a later date.  Official documentation includes a death notice or an original doctor’s certificate identifying the date, length of time expected absence and the specific reason for the absence.  Examinations missed without official documentation and approval result in a grade of zero.
  • There are no deferred options for missed tests.  The value of missed tests, at the discretion of the Faculty, will be added to other evaluation components

English Proficiency
  • All written work should demonstrate the following characteristics for clarity and conciseness:
-writing is consistent with the rules of English grammar
-spelling and punctuation are correct
-sentences are structured correctly
-main ideas are supported with specific, relevant examples and reasons
-work flows logically through supporting statements/paragraphs
-work is arranged in correct format (e.g., as a report, essay)
-up to 10% of the final grade may be deducted on all work if the above English competencies are not met.

Format for Assignments
  • Students must use the standard, APA style for quoting sources.   Help is available at:  http://library.senecacollege.ca

LAB COURSES
Laboratory Attendance

The laboratory component is essential and therefore it is strongly recommended  that you attend all labs.  Any missed labs must be supported with a legal document with three days of the lab.  Any student who fails to attend 2 scheduled laboratory classes for a 7 week subject and more than 3 laboratory classes for a 14 week subject will not pass the subject.    

Laboratory Safety
Students are required to review and understand the safety procedures and guidelines outlined on the first class and sign the sheet to this effect before beginning work in the laboratory.  Students must also wear a lab coat and safety glasses when conducting experiments.
A student who arrives without the proper safety equipment will not be permitted to participant in the lab but will be asked to leave the class.  The student will receive no grade for the lab missed.

Grading is based on the following marking scheme:
Labs (2 at 20% each) 40%
Quiz 10%
Lab Skills 10%
Final Exam  40%

Note: Two Labs (experimental reports) each worth 20% of final mark. The requirements of the reports are presented in writing at the beginning of the class.

*NOTE: TEST AND ASSIGNMENT DATES WILL BE CONFIRMED BY THE INSTRUCTOR

Other Evaluation Considerations
The student is expected to comply with the Safety Rules for working in the laboratory, sign the safety contract, and WILL NOT UNDER ANY CIRCUMSTANCES WEAR CONTACT LENSES in the laboratory.  The student will know where all safety equipment is located in the laboratory and will be familiar with WHMIS concepts and signage.

PLEASE RETAIN THIS SUBJECT OUTLINE FOR POSSIBLE FUTURE USE IN SUPPORT OF CREDIT APPLICATIONS AT OTHER EDUCATIONAL INSTITUTIONS

Approved by: Denis Gravelle