Today’s analytical laboratory is faced with tight deadlines to produce results from testing environmental samples. Too often, solid-phase extraction (SPE) presents a bottleneck in the analytical testing process and may cause poor analyte recoveries and highly variable. Despite advances in analytical instrumentation, sample prep often relies on tedious, manual, and expensive techniques such as liquid-liquid extraction. Sample preparation of environmental water samples can be automated, however.. Use of automated sample preparation addresses the many challenges that laboratories face when preparing samples and can help improve sample processing turnaround times. Chromatography presentation goes with this free on-demand webinar. Link to webinar: https://event.on24.com/eventRegistration/EventLobbyServlet?target=registration.jsp&eventid=832348&sessionid=1&key=7401504685427A0804ABBD1F956E617C&partnerrefthermo=undefined&sourcepage=register

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Automated SPE for the Environmental Testing
Laboratory
Aaron Kettle
Product Manager – Thermo Fisher Scientific,
Automated SPE Systems
9/24/2014
The world leader in serving science

2. The Challenge for Analysis
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1.5 mL GC / LC Vial
How do we get analytes out of these samples?

3. The Answer is Sample Preparation
• Extraction
• Removes analytes from the sample
• Eliminates compounds that interfere with the analysis (Clean Up)
• Evaporation
• Concentrates extracted analytes for analysis
• Evaporates extracted samples for re-constitution
• Most time consuming part of analytical procedure (>60%)*
• Single largest source of errors in the workflow (>30%)**
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*Majors, R.E. LC-GC, 1995, 13, 742-749, and **Majors, R.E. LC-GC, 1999, 17, S8 - S13

4. Analysis Techniques!
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5. Analysis Techniques!
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6. Sample Preparation…
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7. Sample Preparation…
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8. The Important Parameters for Sample Preparation
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• Solvent Use
• Amount of solvent consumed for the extraction
• Solvents are expensive; reducing use reduces costs
• Extraction Time
• Amount of time required for each extraction to occur
• Reducing extraction time increases lab throughput
• % Recovery
• Amount of analyte recovered following the extraction
• Low % recovery yields poor analytical results
• % Relative Standard Deviation (RSD)
• Measure of reproducibility between extractions
• Extraction results have greater reproducibility with lower %RSDs
These Parameters Evaluate SP Techniques

9. Solid-Phase Extraction (SPE)
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• SPE is one of the simplest, most cost-effective and versatile methods of
sample preparation
• SPE has been widely used in many environmental and food laboratories
prior to analysis with GC & GC/MS or LC & LC/MS
• SPE is primarily performed with inexpensive vacuum pumps, manifolds,
and choices of many low-cost, prepackaged, disposable cartridges or
disks.

10. Why is SPE Used?
Concentration
Increases detector
sensitivity and improves
detection limits
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Clean Up
Removes interferences
prior to the analytical
technique Matrix Removal
Removes matrix and elutes
the sample into a solvent
compatible with the analytical
technique

11. SPE vs. Liquid-Liquid Extraction (LLE)
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• Subject to emulsion formation
• Incomplete phase separations
• Poor analyte recoveries
• Uses expensive breakable glassware
• Uses great volumes of solvent
• Must evaporate large volumes of
solvent
• Faster and decreases solvent use
• Can be automated
• More efficient extraction
• Many SPE phases to accomplish
greater separation
• No emulsions
Separatory Funnel used for LLE
Thermo Scientific™ Dionex™ SolEx ™ SPE Cartridges

12. The Process of SPE
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13. Dionex SolEx SPE Sorbent Substrates
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Silica-Based Sorbents Polymeric Sorbents
Silica substrate with bound functional group
Functional group imparts retentive properties
Named for character of the functional group
(e.g. C18)
Styrene-divinyl benzene copolymers that can
be modified to create ion exchangers through
animation or sulfonation
High-capacity particles (800 m2/g) with narrow
size (22 μm) to produce highly efficient low
back-pressure extractions
Activated Carbon
High surface area (1000 m2/g) ensures
retention of multiple analytes simultaneously
High capacity particles (60 μm) ensures
efficient retention in more challenging
matrices (e.g. waste water)

14. Thermo Scientific Dionex AutoTrace 280 SPE Instrument
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47 mm Disk System Cartridge (1, 3 or 6 mL) System
The Thermo Scientific™ Dionex™ AutoTrace 280 SPE instrument provides reliable
automated SPE for analytical chemists determining organic pollutants in large-volume
aqueous samples. Unlike traditional methods such as liquid-liquid extraction using
separatory funnels, the Dionex AutoTrace 280 SPE instrument saves time, solvent and
labor ensuring high reproducibility and productivity for analytical laboratories. The unit can
process up to 6 samples in 2-3 hours.

15. Dionex AutoTrace 280 SPE: For Liquid Samples
• Reduced sample extraction cost
• Solvent consumption (up to 90% less than LLE)
• Labor cost (15 min operator intervention)
• Improved productivity
• 6 samples loaded onto cartridges in 15 min
• Improved analytical precision
• Automated sample loading and elution
• Positive pressure displacement
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6 mL Cartridge System

16. Pesticide Recovery Study
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Dionex AutoTrace 280 SPE instrument Produces Higher Recoveries
than Vacuum Manifold

17. Dionex AutoTrace 280 SPE Instrument
Key Applications Summary
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Analytes Determinative Step Matrix Application Note
Polyaromatic Hydrocarbons
(PAHs)
GC-MS Surface Water AN 876
Dioxins and Furans GC-MS Surface Water AB 805
Polychlorinated Biphenyls
(PCBs)
GC-ECD Surface Water AB 805
Endocrine Disruptors GC-MS
Surface Water
Drinking Water
AB 801
Semivolatile Organic
Compounds
GC & GC-MS Drinking Water AN 819
Organochlorine Pesticides GC-ECD Drinking Water AN 1004
Sex Hormones HPLC-UV Drinking Water TN 148
Tricolsan HPLC-UV Drinking Water AN 1081
Explosives HPLC-UV Ground Water AN 358
Linear Alkyl Benzene Sulfonate HPLC-UV Waste Water AN 1080
Organophosphorous Pesticides GC-NPD Drinking Water Pending Publication
Visit thermoscientific.com/samplepreparation

18. U.S. EPA SPE 500 Methods
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EPA Method Analytes Extraction and Analytical Methods Chemistry Used
506 Phthalate and Adipate Esters SPE and GC/PID C18
507 N and P containing Pesticides SPE and GC C18
508.1
Chlorinated pesticides, herbicides and
organohalides
SPE and GC-ECD C18
521 Nitrosamines SPE and GC/MS/MS Carbon
522 Dioxane SPE and GC/MS Carbon
525.2 Semivolatile Organic Compounds (SVOC) SPE and GC/MS C18
525.3 Semivolatile Organic mpounds (SVOC) SPE and GC/MS C18
526 Semivolatile Organic in DW SPE and GC/MS HRPHS
527 Flame Retardants SPE and GC/MS HRPHS
528 Phenols SPE and GC/MS HRPHS
529 Explosives SPE and GC/MS HRPHS
532 Phenylurea SPE and HPLC C18
535 Acetic Herbicides SPE and LC/MS/MS Graphitized carbon
548 Endothal SPE and GC/ECD C18
539 Hormones SPE and LC/MS/MS HRPHS
553 Benzidines and N containing Pesticides SPE and LC/MS C18
554 Carbonyl compounds SPE and LC C18

19. U.S. EPA SPE 600 /1600 Methods
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EPA Method Analytes Extraction and Analytical Methods Chemistry Used
606,608, 609,
611, 612
Organochlorine Pesticides and PCB’s SPE and GC/ECD C18
1613 Dioxins and Furans SPE and GC/MS C18
1614 Brominated Diphenyl Ehters SPE and HRGCMS C18
1657 Organophosphorous Pesticides GPC/SPE and GC C18
1668a PCB and congeners SPE and HRGC/HRMS C18
1694 Pharmaceuticals & Personal Care Products SPE and LC/MS/MS HRPHS