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 - Gas Chromatography
5 - Supercritical Fluid
6 - Green Chemistry
Instructor(s): Doug Raynie Course Number: 98
Affiliation: South Dakota State University
Course Date: 03/09/2017 - Thursday Course Length: 1 Day Course
Start Time: 08:30 AM End Time: 05:00 PM
Fee: $575 ($775 after 2/18/17) 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, primarily focusing on sample preparation prior to chromatography. Upon successful completion of the course, the participant will have an understanding of sampling considerations 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
(1) General Principles
(2) Trends in Sample Preparation

SAMPLING
(1) Types of Samples
(2) Sample Size Selection
(3) Sample Size Reduction
(4) Particle Size Reduction

GENERAL EXTRACTION CONSIDERATIONS
(1) Thermodynamic Properties
(2) Kinetics
(3) Classification of Methods According to Properties

EXTRACTION FROM LIQUID SAMPLES
(1) Distribution Ratio
(2) Batch Methods: Liquid-Liquid Extraction, Solvent Selection, and Microscale Methods
(3) Continuous Methods
(4) Sorptive Methods: Solid-Phase Extraction, QuEChERS, Solid-Phase Microextraction, and Related Methods
(5) Membrane Methods

EXTRACTION FROM SOLID SAMPLES
(1) General Principles
(2) Soxhlet and Modified Versions
(3) Accelerated Solvent Extraction
(4) Supercritical Fluid Extraction
(5) Microwave-Assisted Extraction
(6) Ultrasound Extraction

TISSUE EXTRACTIONS
(1) Protein Precipitation
(2) Tissues
(3) Matrix-Solid Phase Dispersion

EXTRACTION OF VOLATILE ANALYTES
(1) State and Dynamic Headspace Sampling
(2) Purge and Trap
(3) Thermal Desorption

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

GENERAL LABORATORY PRACTICES
(1) Centrifugation
(2) Gas Cylinders
(3) Glass Handling: Volumetric Glassware, Pipettes, Syringes
(4) Weighing
(5) Filtration
(6) Homogenization
(7) Digestion

POST-EXTRACTION SAMPLE HANDLING
(1) Sample Clean-up
(2) Solvent Drying
(3) Solvent Evaporation
(4) Derivatization

Course Instructor's Biography
Dr. Douglas E. Raynie is an Associate Professor and Department Head in the Department of Chemistry and Biochemistry at South Dakota State University and serves as Sample Preparation Perspectives Editor for LC/GC magazine. 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), alternative solvents, chromatography theory, green analytical chemistry, and problem-based learning in analytical chemistry.