Short Course Listings
 
Short Course

Course Information
Course Title: Analytical Sampling and Sample Preparation
Categories: 1 - Liquid Chromatography
2 - Environmental Analysis
3 - Sample Preparation
4 - Food
5 - Gas Chromatography
6 - Supercritical Fluid
Instructor(s): Doug Raynie Course Number: 109
Affiliation: South Dakota State University
Course Date: 03/01/2014 - Saturday Course Length: 1 Day Course
Start Time: 08:30 AM End Time: 05:00 PM
Fee: $500 ($710 after 2/10/14) 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. The heart of the course will be the presentation of traditional and newly developed chemical extraction methods for sample preparation. Throughout the course both practical and theoretical aspects of the outlined topics and application case studies will be presented.

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

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

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

(The following material is presented in the course notes, but not during the course discussion.)
STATISTICAL CONSIDERATIONS
Statistics
Significant Figures
Accuracy & Precision
Errors
Reference Standards
Uncertainty
Quantitative Methods
External Standard
Internal Standard
Standard Addition
Qualification and Validation

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

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

Course Instructor's Biography
Dr. Douglas E. Raynie is a Research Assistant 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. His undergraduate degree is from Augustana (South Dakota) College, with majors in chemistry and biology. Analytical separations research in Dr. Raynie’s laboratory includes high-resolution chromatography (high-temperature LC and SFC), chromatographic sample preparation (ASE, SFE, SPME, and SPE), chromatography theory, green analytical chemistry, and problem-based learning in analytical chemistry.