Slide 1: An Agilent Guide to SPME Analysis
An Agilent Guide to SPME Analysis Jessica Westland Sample Preparation Application Scientist March 26, 2020 1 An Agilent Guide to SPME Analysis; DE.222337963
Slide 2: Agilent offers high-quality products for SPME sample preparation
Agilent offers high-quality products for SPME sample preparation 2 An Agilent Guide to SPME Analysis; DE.222337963
Slide 3: What is Solid Phase Microextraction (SPME)
What is Solid Phase Microextraction (SPME) Sample preparation technique Solid Phase Microextraction (SPME) is a fast, solvent-less sample extraction technique. It is used for extracting organics from a matrix (solid, liquid, or gaseous) into or onto a stationary phase immobilized on a fiber. In SPME
Slide 4: Parts of the SPME Fiber/Arrow
Parts of the SPME Fiber/Arrow SPME characteristics 4 An Agilent Guide to SPME Analysis; DE.222337963
Slide 5: Key Component – The Phase
Key Component – The Phase SPME fiber hub colors 7 μm PDMS Green 30 μm PDMS Gold 100 μm PDMS Red Acronym Full Name PDMS Polydimethylsiloxane 85 μm Polyacrylate Grey PA Polyacrylate (aka acrylate) DVB Divinylbenzene 95/10 μm CAR-WR/PDMS Dark Blue C-WR Carbon Wide Range 65 μm DVB/PDMS Violet 80/10 μm D
Slide 6: Key Component – The Phase
Key Component – The Phase Acronym PDMS Full Name Polydimethylsiloxane SPME Arrow hub colors PA Polyacrylate (aka acrylate) DVB Divinylbenzene C-WR Carbon Wide Range 100 μm PDMS Red 100 μm Polyacrylate Grey 120 μm CAR WR/PDMS Light Blue 120 μm DVB/PDMS Violet 120 μm DVB/CAR WR/PDMS Dark Grey 250 μm P
Slide 7: SPME Functionality
SPME Functionality 7 An Agilent Guide to SPME Analysis; DE.222337963
Slide 8: Fiber/Arrow Conditioning
Fiber/Arrow Conditioning SPME functionality Fibers/Arrows MUST be preconditioned prior to first use (or after sitting) • Done at a specified temperature in an inert gas phase environment (He or N2) Fibers/Arrows MUST be conditioned prior to and/or after desorption of sample – cleans the fiber • Done
Slide 9: Manual Sampling
SPME Manual Sampling SPME functionality The Agilent manual injection kit (p/n 5191-5877) will allow the end user to extract samples using SPME fibers or arrows and then inject the samples into a GC inlet. Part Component 1 Extraction guide 2 Injection guide 3 Arrow/fiber syringe 4 Large inner diamete
Slide 10: Manual Sampling
SPME Manual Sampling Agilent demonstration guide: 5994-1732EN Manual SPME sampling: SPME fibers and Arrows A detailed step-by-step guide (with images) to assist with the installation of a SPME fiber or Arrow into the manual sampling holder for either headspace or immersion sampling and adjustments f
Slide 11: Automated Sampling
SPME Automated Sampling SPME functionality Agilent’s SPME fibers and Arrows work directly with your current rail system. PAL-xt Holder PAL SPME tool PAL SPME fiber tool PAL SPME Arrow tool For PAL and PAL-xt systems For older PAL system PAL3 Series RSI and PAL3 Series RSI and with CombiPAL and PAL M
Slide 12: Automated Sampling: Changes for SPME Arrows
SPME Automated Sampling Changes for SPME Arrows Due to their larger diameter, SPME Arrows require instrumental changes in addition to obtaining the SPME Arrow option on the PAL3 rail system. You need an enlarged GC turn top assembly You must use an inlet liner with a larger diameter 0.75 mm id 2 mm
Slide 13: SPME Applications
SPME Applications 13 An Agilent Guide to SPME Analysis; DE.222337963
Slide 14: Sampling
SPME Sampling Applications Intensity Equilibrium condition • Sorbent material • Temperature • Time Kinetics influence • Stirring/agitation • Salting out Time control critical for • pH Value quantitation, needs auto-sampling • Temperature Supelco 2011 - Michel, F., Buckendahl, K., Basics in Solid Pha
Slide 15: Sampling – Salting out
SPME Sampling – Salting out Applications Arrow 120 μm CAR WR/PDMS Black trace – with NaCl at 3 ppb Blue trace – without NaCl at 3 ppb 15 An Agilent Guide to SPME Analysis; DE.222337963
Slide 16: Fiber or Arrow
SPME Fiber or Arrow Applications Intensity Speed • Shorter extraction speed • For same response as fibers SPME Arrow – Improved productivity – Higher sample throughput SPME fiber Sensitivity • Higher response • At same extraction time as fibers – Lower detection limits – Improved precision Extra
Slide 17: Fiber or Arrow
SPME Fiber or Arrow Applications 5 ppb BTEX with 5 min incubation and 3 min extraction Black trace – Arrow Blue trace – fiber 17 An Agilent Guide to SPME Analysis; DE.222337963
Slide 18: Analyte Relation to Phase Type
Analyte Relation to Phase Type Applications 7 μm PDMS Thinner coatings For higher MW compounds Can accept higher conditioning temperature 30 μm PDMS Absorbent 100 μm PDMS 85 μm Polyacrylate 95/10 μm CAR-WR/PDMS Thicker coatings Require longer extraction times 65 μm DVB/PDMS Adsorbent Use lower condi
Slide 19: Analyte Relation to Phase Type
Analyte Relation to Phase Type Applications Nonpolar high MW compounds 7 μm PDMS Nonpolar semi-volatiles 30 μm PDMS Nonpolar Volatiles 100 μm PDMS Polar semi-volatiles 85 μm Polyacrylate Polar Gases and volatiles 95/10 μm CAR-WR/PDMS Polar volatiles 65 μm DVB/PDMS Bipolar Odors and flavors 80/10 μm
Slide 20: Examination of Lower Molecular Weight PAHs in Drinking Water Using Agilent PDMS SPME Fibers
Examination of Lower Molecular Weight PAHs in Drinking Water Using Agilent PDMS SPME Fibers Learn more, search 5994-1301EN at www.agilent.com Polycyclic aromatic hydrocarbons (PAHs) are a large class of organic compounds containing two or more fused aromatic rings. PAHs are considered compounds of c
Slide 21: Analysis of BTEX in Water with a CAR-WR/PDMS SPME Fiber
Analysis of BTEX in Water with a CAR-WR/PDMS 95 μm SPME Fiber Learn more, search 5994-1104EN at www.agilent.com The production of safe drinking water is an important issue, and legislation has established allowed levels of chemical substances in drinking water, whether they occur naturally, as delib
Slide 22: Determination of VOCs in Water by GC/MS after HS-SPME
Determination of VOCs in Water by GC/MS after Headspace-Solid-Phase Microextraction (HS-SPME) Learn more, search 5994-1045EN at www.agilent.com The addition of NaCl increased the extraction efficiency for the analytes of interest. Chromatogram of 0.8 ppb BTEX standard analyzed by a 120 μm CAR WR/PDM
Slide 23: SPME-GC/MS of Selected Terpenes using Agilent DVB/CAR-WR/PDMS SPME Fiber
SPME-GC/MS of Selected Terpenes using Agilent DVB/CAR-WR/PDMS SPME Fiber Learn more, search 5994-1411EN at www.agilent.com Since terpenes have high vapor pressures, and are extremely volatile, they are excellent candidates for static headspace (HS) gas chromatography/mass spectrometry (GC/MS) analys
Slide 24: SPME Arrow Sampling of Terpenes in Cannabis Plant Material
SPME Arrow Sampling of Terpenes in Cannabis Plant Material Learn more, search 5994-1046EN at www.agilent.com PAL SPME Arrows provided the sensitivity and robustness needed to profile the predominant terpenes in an unknown variety of cannabis plant samples Flower sample 3812 Flower sample 3813 Flower
Slide 25: Analysis of Parathion-Ethyl in Water with a Polyacrylate SPME Fiber
Analysis of Parathion-Ethyl in Water with an 85 μm Polyacrylate SPME Fiber Learn more, search 5994-1546EN at www.agilent.com Organophosphorus insecticides are among the most widely used pesticides throughout the world. As a result of their widespread use their residues have been detected in samples
Slide 26: Immersion Sampling Best Practices
Immersion Sampling Best practices • Immersion sampling sensitivity is improved by filling the sampling vial to a minimum of 80% • Immersion sampling works best for low concentration water-based sample matrices • When using immersion for samples containing sugars, proteins, and particulate matter, ri
Slide 27: SPME-GC/MS of 2,4,6-trichloroanisole Using Agilent DVB/PDMS SPME Fiber
SPME-GC/MS of 2,4,6-trichloroanisole Using Agilent DVB/PDMS SPME Fiber Learn more, search 5994-1564EN at www.agilent.com The main compound responsible for cork taint is 2,4,6-trichloroanisole. It is one of the most odor intense compounds known and has a distinct musty, moldy aroma. 2,4-Dichloroaniso
Slide 28: SPME Troubleshooting
SPME Troubleshooting Make troubleshooting faster and easier by closely observing and keeping complete records of your analytical methodologies 28 An Agilent Guide to SPME Analysis; DE.222337963
Slide 29: Needle Bends/Fiber Breaks
Needle Bends/Fiber Breaks SPME troubleshooting Improper alignment is one of the main causes of fiber/arrow damage. • Follow Agilent’s Demonstration Guide (5994-1732EN) to ensure proper alignment and set up of the manual sample holder • Retract fiber into protective needle during insertion into vial/
Slide 30: Septum Issues
Septum Issues SPME troubleshooting Septum of sample vial cap is too thick • Use on Agilent screw headspace magnetic caps (p/n 5188-2759; 18 mm) PTFE/silicone septa (top white, bottom blue) on Agilent amber screw top headspace sampling vials (p/n 5188-6537; 20 mL) Septum in injection port is too thic
Slide 31: Discolored Coatings
Discolored Coatings SPME troubleshooting Coatings will discolor when heated too high or there are leaks in the flow path • Minimize oxygen in carrier gas, condition fibers in oxygen free gas flow – p/n CP17970: Gas Clean oxygen purifier – p/n CP17973: Gas Clean carrier gas purifier • Reduce the inje
Slide 32: Data Analysis
Data Analysis SPME troubleshooting Endogenous peaks in chromatogram • Precondition fiber/arrow prior to sampling • Use low-bleed septa to minimize injection port septum bleed or a septum-less injector system (i.e. Merlin Microseal) • Replace the inlet liner Interfering peaks • Change GC column or te
Slide 33: SPME Summary
SPME Summary Solid phase microextraction (SPME) Agilent offers high-quality products for SPME sample preparation Agilent puts together the supplies for both manual and automated SPME sampling Agilent follows the market trends to keep you up to date with application notes and technical collateral 33
Slide 34: Columns, Sample Prep and Supplies Questions
Columns, Sample Prep and Supplies Questions Do you have questions about the following during a potential lab shutdown? • Column storage • What to do with mobile phase, buffers, and other HPLC solvents • Chemical standards storage • What supplies to stock up on to get your instrument back up and runn
Slide 35: Contact Agilent Chemistries and Supplies Technical Support
Contact Agilent Chemistries and Supplies Technical Support 1-800-227-9770 Option 3, Option 3: Option 1 for GC/GCMS Columns and Supplies Option 2 for LC/LCMS Columns and Supplies Option 3 for Sample Preparation, Filtration and QuEChERS Option 4 for Spectroscopy Supplies Option 5 for Chemical Standard
Slide 36: Looking to increase your knowledge during your lab shutdown?
Looking to increase your knowledge during your lab shutdown? Check out on-demand and live webinars on GC/GCMS, LC/LCMS and Sample Prep consumables. https://www.agilent.com/en/training-events/eseminars/gc-gc-ms-webinars https://www.agilent.com/en/training-events/eseminars/lc-lc-ms-column-e-seminars 3
Slide 37: Thank You
Thank You 37 An Agilent Guide to SPME Analysis; DE.222337963