Course Information
Course Title: Sampling and Sample Preparation
Categories: 1 - Liquid Chromatography
2 - Environmental Analysis
3 - Sample Preparation
4 - Gas Chromatography
5 - Supercritical Fluid
Instructor(s): Doug Raynie Course Number: 91
Affiliation: South Dakota State University
Course Date: 03/11/2012 - Sunday Course Length: 2 Day Course
Start Time: 08:30 AM End Time: 05:00 PM
Course Date 2: 03/12/2012 - Monday    
Start Time: 08:30 AM End Time: 05:00 PM
Fee: $900 ($1300 after 2/13/12) Textbook Fee:

Course Description
This short course is designed to provide participants with an in-depth understanding of the role of sampling and sample preparation in analytical chemistry. Upon successful completion of the course, the participant will have an understanding of sampling consideration and approaches, and sample preparation strategies. The course will begin by discussing the role of sampling, sample types, sample size, sample storage and handling, etc. Next, general laboratory skills that are often overlooked, but which greatly impact the overall analysis, will be reviewed. The heart of the course will be the presentation of traditional and newly developed chemical extraction methods for sample preparation. Finally, post-extraction sample treatment will be addressed. Throughout the course practical and theoretical aspects of the outlined topics and application case studies will be presented. PLEASE BRING FLASH DRIVE FOR ON-SITE UPDATES TO COURSE.

Target Audience
This short course is intended for both bench and supervisory chemists responsible for the method development and analytical extraction of samples prior to gravimetric, chromatographic, or spectroscopic determination.

Course Outline
INTRODUCTION
General Principles
Trends in Sample Preparation
STATISTICAL CONSIDERATIONS
Statistics
Significant Figures
Accuracy & Precision
Errors
Reference Standards
Uncertainty
Quantitative Methods
External Standard
Internal Standard
Standard Addition
Qualification and Validation

SAMPLING
Types of Samples
Sample Size Selection
Sample Size Reduction
Particle Size Reduction

GENERAL LABORATORY PRACTICES
Centrifugation
Gas Cylinders
Glass Handling
Volumetric Glassware, Pipettes, Syringes
Weighing
Filtration
Homogenization
Digestion

GENERAL EXTRACTION CONSIDERATIONS
Thermodynamic Properties
Kinetics
Classification of Methods According to Properties

EXTRACTION FROM LIQUID SAMPLES
Distillation Methods
Batch Methods
Liquid-Liquid Extraction
Micro-Liquid-Liquid Lxtraction
Single-Drop Microextraction
Solvent Sublation
Continuous Methods
Continuous Liquid-Liquid Extraction
Countercurrent Extraction
ExCell
Sorptive Methods
Solid-Phase Extraction
Solid-Phase Microextraction
Stir-Bar Sorptive Extraction
Membrane Methods
Classification of Methods
Dialysis and Microdialysis
Supported-Liquid Membrane Extraction

EXTRACTION FROM SOLID SAMPLES
General Principles
Shake-Flask
Soxhlet and Automated Soxhlet
Forced-Flow Leaching
Accelerated Solvent Extraction
Supercritical Fluid Extraction
Microwave-Assisted Extraction
Ultrasound Extraction
Method Comparison

CHEMICAL EXTRACTIONS – SPECIAL CASES
Inorganics
Tissues

EXTRACTION OF VOLATILE ANALYTES
Headspace Sampling
Static
Dynamic
Purge and Trap
Thermal Desorption

POST-EXTRACTION SAMPLE HANDLING
Sample Clean-up
Solvent Drying
Solvent Evaporation
   Derivatization

Course Instructor's Biography
Dr. Douglas Raynie is a Research Associate Professor in the Department of Chemistry and Biochemistry at South Dakota State University. Prior to joining SDSU, he was employed for eleven years as a Senior Scientist at Procter and Gamble's Corporate Research Division. He earned his Ph.D. at Brigham Young University under the direction of Dr. Milton L. Lee. Dr. Raynie’s research interests include high-resolution chromatography (including high-temperature LC and SFC), chromatographic sample preparation (including ASE, SFE, SPME, and SPE), chromatography theory, green chemistry, and problem-based learning in analytical chemistry. At P&G, he introduced ASE to industry as one of the world's first practitioners of the technique. Dr. Raynie has served on the editorial advisory boards of the Journal of Microcolumn Separations and the Encyclopedia of Separation Science. He is a member of the American Chemical Society (Division of Analytical Chemistry and Subdivision on Chromatography), the American Association for the Advancement of Science, and the International Society for the Advancement of Supercritical Fluids.