Course Information
Course Title: Headspace Analysis - Theory and Practice
Categories: 1 - Pharmaceutical Sciences
2 - Clinical Analysis
3 - Polymers
4 - Sample Preparation
5 - Food
6 - Gas Chromatography
Instructor(s): Michael Markelov Course Number: 111
Affiliation: ACS Labs
Course Date: 03/10/2012 - Saturday Course Length: 2 Day Course
Start Time: 08:30 AM End Time: 05:00 PM
Course Date 2: 03/11/2012 - Sunday    
Start Time: 08:30 AM End Time: 05:00 PM
Fee: $900 ($1300 after 2/13/12) Textbook Fee:

Course Description
This two-day short course will concentrate on quantitative aspects of Headspace Analysis. Every theoretical point including the effect of temperatures, salinity, sample volume, etc. will be illustrated by practical examples. Emphasis will be made on the use of Matrix Independent Quantification Techniques. Different Headspace Instruments and Headspace sampling approaches will be presented. Effects of various parameters of sampling like pressurization time, pressure, equilibration time and temperature, agitation techniques, etc. will be demonstrated. Instrumental and procedural parameters important for validation of headspace methods will be addressed. Special attention will be given to the analysis of unstable and solid matrices like food and polymers. The practicum part of the course will teach students to estimate expected sensitivities of Headspace analysis for various analyte/matrix compositions. Please bring a scientific calculator.

Target Audience
This course is suitable for all levels of participants with chemical background. Lab managers will learn about many new applications. Chemists will learn various quantification approaches. Technicians will learn how to recognize instrumental and/ or procedural problems. Chemical engineers will find it very useful for characterization of real plant streams.

Course Outline
Course Topics
Day 1 – Morning
• Introduction section includes:

a. Description of different types of headspace sampling
b. Comparison of static versus purge and trap headspace methods
c. Different types of analytes and matrices that are typical subjects of headspace analysis
d. Typical sensitivities for different analytes in different matrices

• Theory in Action

a. Definition and basic equations
b. Headspace as an extraction technique
c. Matrix effects in GC and Headspace

• Examples and Explanation of Matrix Effects

a. Effect of temperature
b. Effect of salinity
c. Presence of solids
d. Effect of different type of solvents
e. Effect of pH
f. Maximizing sensitivity using all these effects

Day 1- Afternoon

• Calibration and Quantification in Headspace Analysis

a. Calibration of gaseous phase for quantification of odors, explosion and health hazard limits
b. Determination of partial vapor pressures
c. Calibration approaches for analysis of condensed matrices

• Description and Practical use of Matrix Independent Techniques

a. MSA- method of Standard Additions
b. MHE- Multiple Headspace Extraction
c. VPT- Variable Phase Ratio or Variable Volume technique
d. FET – Full Evaporation Technique

• Practicum
a. Calculation of  expected sensitivity for several chemicals in different matrices
b. Calculation of concentrations of chemicals from chromatograms provided
c. Increasing the sensitivity using approaches learned in the earlier sections
d. Evaluation of Headspace parameters for validation purposes

Day 2 – Morning

•  General Principles and Specifics of Instrumentation for Headspace Analysis
(Agilent, EST-9000, Gerstel, LEAP,  Perkin-Elmer,  Teledyne –Tekmar, etc.)
a. Syringe based system 
b. Volume controlled injection 
c. Time controlled injection systems
d. Dual needle sampling
e. Multifunctional Headspace instruments 
f. Some special injection devices

• Selection of Instrumental Parameters

a. Temperature zones
b. Speed and time of pressurization
c. Vial pressure
d. Time and rate of de-pressurization (loop fill)
e. Injection times
f. Trapping parameters

• Validation of Headspace GC Methods


Day 2 – Afternoon

• Specific Applications

a. Environmental analysis
b. Pharmaceuticals
c. Food, Flavors, and Fragrances
d. Biological and Forensic Samples
e. Paints and Latexes
f. Analysis of polymers below and above their glass transition points

• Special and Unusual Applications

a. Derivatization techniques
b. Determination of solubility limits
c. Determination of activity coefficients, enthalpies, free energy, and partial vapor pressure over complex matrices
d. Determination of Partition Coefficients in multi-component solutions

• Optional topics

a. Combination of headspace sampling with non-chromatographic analyzers
 (Electronic Nose, Mercury Analyzer, Infrared, etc.)
b. Process headspace analysis

Course Instructor's Biography
Dr. M. Markelov has been practicing headspace Analysis for more than 25 years and teaching this continuously updated course for more than 15 years. While working as a head of Headspace and Trace Analysis laboratory in the Standard Oil Co. and then British petroleum, he was teaching short headspace courses for polymer chemists and chemical engineers. This course was later expanded on the request of Hewlett Packard and Tekmar companies and given for their customers. Dr. M. Markelov published numerous papers on the subject and holds several patents for headspace instruments.