Sorbent Pens. For Next Generation Headspace Analysis

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1 Sorbent Pens For Next Generation Headspace Analysis

Headspace Sorbent Pens - The Ultimate Extraction Power Introducing Entech s exciting new Sorbent Pen technology.

Sorbent Pens combine the features of SPME and classical ¼ adsorbent traps in a design with far more flexibility and enhanced performance.

The Sorbent Pen is then desorbed directly onto the head of a GC column to eliminate losses associated with standard thermal desorption systems that must transport the desorbed sample through rotary

2 Headspace Sorbent Pens - The Ultimate Extraction Power Introducing Entech s exciting new Sorbent Pen technology. The most versatile extraction and sample preconcentration technology available for GC and GCMS. Sorbent Pens combine the features of SPME and classical ¼ adsorbent traps in a design with far more flexibility and enhanced performance. Sorbent Pens are extremely durable and are designed to perform both active and diffusive sampling. The Sorbent Pen is then desorbed directly onto the head of a GC column to eliminate losses associated with standard thermal desorption systems that must transport the desorbed sample through rotary valves, secondary traps, and a lengthy transfer line prior to delivery onto the GC column. The Sorbent Pen uses an entirely new approach for sample extraction. Direct insertion of the Sorbent Pen into the vial headspace followed by evacuation of the vial through the top of the Pen allows a new technique called "Vacuum Assisted Sorbent Extraction", or VASE, to recover a far wider range of compounds than ever before. With Sorbent Pens, both VOCs and SVOCs can be measured in wastewater, breath condensate, alcoholic beverages, and virtually all other matrices. VASE offers a tremendous advantage over other extraction techniques that perform extractions at atmospheric pressure where diffusion rates are suppressed. Sorbent Pens perform sample enrichment offline from a GCMS, allowing all samples to extract simultaneously and for longer periods of time. This approach results in high throughput while yielding a more complete and reproducible extraction for more sensitive and quantitative measurements. The low cost 5800 Sorbent Pen Desorption Unit (5800 SPDU) makes this exciting new technique both affordable and practical for virtually any laboratory s budget. Then move up to 90 sample automation with the 7800 Autosampler for the ultimate in laboratory productivity. Join the Sorbent Pen movement and take advantage of the next generation in GCMS sample preparation. Improvements over SPME and Dynamic Headspace Trapping Applications include: Cannabis - Pesticide Screening Highly reproducible. - Terpene Profiling Very low carryover. - Potency Testing Durable - hundreds of injections. - CBD, THC Operates at or near equilibrium to improve sensitivity and quantitative accuracy. Perform exhaustive vacuum extraction of VOCs through SVOCs. Unlike SPME, outer sheath minimizes exposure to aerosols formed during agitation. See taints, odors, additives, flavors & fragrances at levels below previously possible. Faster injection rates produces better chromatography / less thermal degradation. Rapid injections without cryogen or electronic cooling. Usually requires no secondary bakeout/cleanup. Higher sensitivity and throughput via off-line extraction. Sample up to days under vacuum for unsurpassed SVOC recovery. Sample at elevated or sub-ambient temperatures as needed. Food Safety - Nitrosamines - Acrylimides - Pesticides/Herbicides - Carcinogens - Preservatives Flavors/Aromas - Foods - Beverages - Alcoholic Beverages Fragrances - Taints/Off-Flavors - Odors in Consumer Products - Residue Drugs/Pharma - PCBs, PBDEs Water Analysis - Odors - SVOCs - VOCs Clinical Markers/Drugs In - Blood - Urine - Breath For a complete list of applications, visit entechinst.com Headspace Sorbent Pens DESCRIPTION PART # UNIT Headspace Sorbent Pens Tenax TA (35/60) SP-HS-T3560 EA Tenax + Carboxen 000 SP-HS-TCBXN EA Empty Headspace Pen SP-HS-0 EA Headspace Pen Tray SP-HS-TRAY30 EA Durable, Reuseable, and Cost Effective!

3 VASE using Sorbent Pens Operates at or Near Equilibrium to Improve Sensitivity and Reproducibility Operating at or near equilibrium increases sensitivity and reduces run to run variability Small movements back and forth on curve for VASE as the samples approach equilibrium causes little change in recoveries, and therefore reproducibility. VASE - Vacuum Assisted Sorbent Extraction 00% Relative Difference -5% At Equilibrium VASE % Recovery (Compound Dependent) Rate of Extraction Is Not As Important If Analysis Is Made After Equilibrium Is Achieved Pen Pen Fiber Fiber 3x x SPME - -0% Recovery Highly Variable Run to Run Requires Isotope Dilution for Quantitation Relative Difference 300% Due To Rate Differences During Extraction Time Equilibrium Reached VASE (Sorbent Pens ) vs SPME and SBSE (Twister ) Recovery Relative to Analyte Volatility Sorbent Pens using Vacuum Assisted Sorbent Extraction (VASE) recover compounds starting even lighter than SPME, and out to nearly those recovered by SBSE Most applications done by either SPME or SBSE can be done more easily and usually with higher sensitivity and accuracy with VASE using Sorbent Pens

Sorbent Pen Desorption Unit (SPDU) Sorbent Pens are analyzed using the 5800 SPDU.

The complete desorption process is performed automatically to transfer both volatile and semi-volatile compounds onto the GCMS for

Control the desorption temperature to either limit or maximize the molecular weight range transferred onto the column.

optimum long-term performance. Methods are created and stored on the same PC operating the GCMS.

4 Sorbent Pen Desorption Unit (SPDU) Sorbent Pens are analyzed using the 5800 SPDU. After sample enrichment, simply insert the Sorbent Pen into the 5800 SPDU, and press START on the 5800 SPDU Controller. The complete desorption process is performed automatically to transfer both volatile and semi-volatile compounds onto the GCMS for extremely sensitive and accurate headspace analysis. Control the desorption temperature to either limit or maximize the molecular weight range transferred onto the column. A unique desorber design utilizes a Silonite coated flow path, allowing simple liner replacement to maintain maximum inertness for optimum long-term performance. Methods are created and stored on the same PC operating the GCMS. Develop methods using this entry level solution and then add the 7800 Autosampler when you are ready to fully automate the analysis of up to 90 Sorbent Pens SPDU Easily transfers volatile and semi-volatile compounds to a GCMS for extremely sensitive and accurate headspace analysis SPDU Ordering Information DESCRIPTION PART # UNIT Sorbent Pen Desorption Unit (0VAC) 5800-SPDU EA Sorbent Pen Desorption Unit (30VAC) 5800-SPDU-HV EA 5800 SPDU Liner for Headspace Sorbent Pen 5800-LNR-HS EA GC Model Mounting Kits: Agilent 6890/7890(B) 5800-GC-AG EA Thermo 300/30 GC 5800-GC-TH EA Shimadzu 00 GC 5800-GC-SH EA 3

5 Sorbent Pen Autosampler The 7800 Autosampler automates the analysis of up to 90 Sorbent Pens using 3 removable 30 position trays. The ability to use Sorbent Pens to pre-extract the headspace in a sample vial, or perform air sampling in almost any location, followed by rapid delivery to a GCMS creates the ideal combination of sensitivity and efficiency. The 7800 delivers each Sorbent Pen to the 5800 SPDU for GCMS injection and bakeout. After bakeout, the 7800 returns the Sorbent Pen to the sealed sample tray leaving clean Pens that are usually ready for resampling without further conditioning. The Sorbent Pen's unique triple o-ring seal ensures leak tight connections, while the design of the 5800 provides rapid and reproducible transfer to the GC column to support quantitative headspace analysis. The combined power and simplicity of the Sorbent Pen and 7800 / 5800 SPDU provides an ideal solution for recovering a vastly extended range of compounds in the sample headspace, allowing development of hundreds of applications compatible with virtually any matrix Sorbent Pen Autosampler Part# 7800-SPA Sorbent Pen Extraction System The Sorbent Pen Extraction System provides a convenient way to perform vial extractions using 30-position trays. Load the sample to be extracted into the vial, insert the Sorbent Pen, create a vacuum through the MicroQT seal at the top of the Pen, and then load the tray into the 5600 to start the vacuum extraction. The Sorbent Pen Extraction System agitates the samples at RPM to speed up transfer of volatiles to the headspace, while heating the sample from ambient +4 C to 70 C. Extractions will be complete in 48 hours depending on the application. DESCRIPTION PART # UNIT 5600 Sorbent Pen Extraction System 5600-SPES EA 5600 Sorbent Pen Extraction System (30VAC) 5600-SPES-HV EA 30-Position Tray for 0/40/60 ml Vials TRAY30 EA 30-Position Tray for 5mL Vials TRAY30 EA 40mL Clear Vials pk 0mL Clear Vials pk Extraction Lid for 40mL Vial / 5mL Bottle SP-L04S EA Plastic Vial Caps (40mL/5mL) B 44pk Dual Stage Diaphram Pump EA Dual Stage Diaphragm Pump (30VAC) EA Vial Evacuation Unit SP-VIAL-EVAC EA 4

3 Sorbent Pen Thermal Conditioner The 380 can be used to condition Sorbent Pens prior to use at temperatures up to 350 C.

concentrations where complete removal of the residual sample did not occur during the previous analysis.

an internal valve starts and stops the flow of UHP Nitrogen at appropriate Sorbent Pen conditioning temperatures.

6 3 Sorbent Pen Thermal Conditioner The 380 can be used to condition Sorbent Pens prior to use at temperatures up to 350 C. Use the 380 for new Pens, Pens that were not isolated after desorption, and Pens that contained unusually high concentrations where complete removal of the residual sample did not occur during the previous analysis. Flow rate of thermal conditioning gas is controlled and monitored through a convenient front panel flow controller, while an internal valve starts and stops the flow of UHP Nitrogen at appropriate Sorbent Pen conditioning temperatures. 380 Sorbent Pen Thermal Conditioner DESCRIPTION PART # UNIT Sorbent Pen Thermal Conditioner (0VAC) 380-SPTC EA Sorbent Pen Thermal Conditioner (40VAC) 380-SPTC-HV EA 5

Headspace Bundle Kit 5800 SPDU Injector Unit 5800 SPDU

Sorbent Pens 30 Position Tray for Headspace Sorbent Pens

Lid Cap Sorbent Pen Thermal Conditioner Sorbent Pen Extraction

pos tray for 40mL vials L Clear Vial -Stage Oilless Diaphragm

5800-SPDU EA 5800 Liner for Headspace Sorbent Pen 5800-LNR-HS

SP-HS-0 EA 30 Position Tray Headspace Sorbent Pens SP-HSTray30

30-0 Hg Vacuum Test Gauge (W/ Micro-QT ) 9-7000QT EA

EA 30 Position Tray for 40mL Vials 5600-040TRAY30 EA 40mL Clear

Vials/5mL Bottles SP-L04S EA Low Bleed Blue Viton O-Rings

7 Headspace Bundle Kit 5800 SPDU Injector Unit 5800 SPDU Controller Vial Evacuation Unit 5800 Liner for Headspace Sorbent Pens 30 Position Tray for Headspace Sorbent Pens Sorbent Pen L Extraction Vial Kit Fitting Cap Sorbent Pen Lid Lid Cap Sorbent Pen Thermal Conditioner Sorbent Pen Extraction System SP-HS-B0 Headspace Bundle Kt 40mL & 0mL Clear Vial 30 pos tray for 40mL vials L Clear Vial -Stage Oilless Diaphragm Pump DESCRIPTION PART # UNIT Sorbent Pen Desorption Unit 5800-SPDU EA 5800 Liner for Headspace Sorbent Pen 5800-LNR-HS EA Tenax HS Sorbent Pen SP-HS-T3560 EA Blank HS Sorbent Pen SP-HS-0 EA 30 Position Tray Headspace Sorbent Pens SP-HSTray30 EA -Stage Oilless Diaphragm Pump EA PDMS Pre-Column (5m x 0.5mm ID, 0.5um) EA Sorbent Pen Thermal Conditioner 380-SPTC EA 30-0 Hg Vacuum Test Gauge (W/ Micro-QT ) QT EA DESCRIPTION PART # UNIT Sorbent Pen Extraction System 5600-SPES EA 30 Position Tray for 40mL Vials TRAY30 EA 40mL Clear Vials pk 0mL Clear Vials pk Lid for 40/60mL Vials/5mL Bottles SP-L04S EA Low Bleed Blue Viton O-Rings SP-L04-OR 0pk Caps for 40/60mL Vials/5mL Bottles B 44pk L Sorbent Pen Extraction Vial Kit with Lid/Cap/Fitting SP-HS-VL EA Vial Evacuation Unit SP-VIAL-EVAC EA 6

Brie Cheese Duplicate Analysis.e+07 e+07 9000000 8000000 7000000 6000000 5000000 4000000 SORBENT PEN # 8 3 3000000 000000 000000 0 3 4 5 6 7 9 0 3 4 5 6 7 8 0.00 5.00 0.00 5.00 30.00 35.00 9 *0 4.

00 7 8 9 *0 4 *Difference in Dodecanoic acid, ethyl ester caused by difficulty in maintaining exact amount of cheese sample oxidation from run to run, and expected variations in sample homogeneity.

8 Brie Cheese Duplicate Analysis.e+07 e SORBENT PEN # *0 4.e+07 e SORBENT PEN # *0 4 *Difference in Dodecanoic acid, ethyl ester caused by difficulty in maintaining exact amount of cheese sample oxidation from run to run, and expected variations in sample homogeneity. Instrument: Run date: Sample description: Weight of sample (g): Sample conditions: Desorb conditions: Split Mode: Precolumn: Column: Carrier: Oven Temp: GCMS: MS Operation: 5800 HSP 5-Aug-6 Brie 70g cheese in 40mL water, blended, 0.05g taken blended + vac(30sec) + 50 C + 3 hr equilibration 60 C for 5 min. Splitless DB 5m length x 0.5mm ID, 0.5µm film DB 30m length x 0.5mm ID, 0.5µm film He,.5cc/min. constant flow 40 C hold 5min., 6 C/min. to 95 C, 0 C/min. to 40 C, 0 C/min. to 35 hold 5min. Agilent 7890B/5977A amu,.8 scans/sec. 4-Heptanone. -Heptanone 3. Benzaldehyde 4. -Octanone 5. Hexanoic acid, ethyl ester 6. Benzeneacetaldehyde 7. 8-Nonen--one 8. -Nonanone 9. Nonanal 0. Octanoic acid. Octanoic acid, ethyl ester. Decanal 3. n-octanoic acid isopropyl ester 4. -Undecanone 5. n-decanoic acid 6. Decanoic acid, ethyl ester 7. H-Pyran--one, tetrahydro-6-pentyl- 8. -Tridecanone 9. Dodecanoic acid 0. Dodecanoic acid, ethyl ester. H-Pyran--one, 6-heptyltetrahydro-. Tetradecanoic acid 3. n-hexadecanoic acid 4. Hexadecanoic acid, ethyl ester 7

Extremely Clean Blank After Strawberry Analysis 9 3.5e+08 3e+08.5e+08 e+08.5e+08 e+08 5e+07 0 4 8 6 5 0 3 5 7 34 8 7 9 6 6.00 8.00 0.00.00 4.00 6.00 8.00 0.00.00 4.00 6.00 8.00 3.

9 Extremely Clean Blank After Strawberry Analysis 9 3.5e+08 3e+08.5e+08 e+08.5e+08 e+08 5e e+08 3e+08 Blank run of the same Sorbent Pen directly after strawberry sample.5e+08 e e+08 e+08 5e Instrument: Run date: Sample description: Weight of sample (g): Sample conditions: Desorb conditions: Split Mode: Precolumn: Column: Carrier: Oven Temp: GCMS: MS Operation: 5800 HSP 3-Aug-6 Fresh strawberries vac(30sec) + 5hr equilibration 60 C for 5 min. Splitless DB 5m length x 0.5mm ID, 0.5µm film DB 30m length x 0.5mm ID, 0.5µm film He,.5cc/min. constant flow 40 C hold 5min., 6 C/min. to 95 C, 0 C/min. to 40 C, 5 C/min. to 35 hold 5min. Agilent 7890B/5977A amu,.8 scans/sec Ethyl acetate. Butanoic acid methyl ester 3. Propanoic acid, -methyl-, ethyl ester 4. Butanoic acid, ethyl ester 5. Acetic acid, butyl ester 6. Butanoic acid, -methyl-, ethyl ester 7. -Butanol, 3-methyl-, acetate 8. Hexanoic acid, methyl ester 9. Hexanoic acid, ethyl ester 0. -Hexen--ol, acetate, (Z)-. 3(H)-Furanone, 4-methoxy-,5-dimethyl-.,6-Octadien-3-ol, 3,7-dimethyl- 3. Octanoic acid, methyl ester 4. Methyl salicylate 5. Octanoic acid, ethyl ester 6. Butanoic acid, octyl ester 7. Pentanoic acid, octyl ester 8.,6,0-Dodecatrien-3-ol, 3,7,-trimethyl- 9..gamma.-Dodecalactone Zoomed in baseline still reveals a completely clean chromatogram

Dark Chocolate Analysis.5e+08.4e+08.3e+08 4.e+08.e+08 e+08 9e+07 5 36 8e+07 7e+07 6e+07 5e+07 3 4e+07 6 9 33 3e+07 0 e+07 9 5 3 7 8 30 e+07 3 34 35 37 38 39 40 0.00 5.00 0.00 5.00 30.00 35.

Split Mode: Precolumn: Column: Carrier: Oven Temp: GCMS: MS Operation: Pen ID: 5800 HSP 7-Nov-6 Dark Chocolate 40 ml vial + vac(30sec) + 5hr equilibration @ 5C 60 C for 5 min.

10 Dark Chocolate Analysis.5e+08.4e+08.3e+08 4.e+08.e+08 e+08 9e e+07 7e+07 6e+07 5e e e+07 0 e e Instrument: Run date: Sample description: Amount of sample (g): Sample conditions: Desorb conditions: Split Mode: Precolumn: Column: Carrier: Oven Temp: GCMS: MS Operation: Pen ID: 5800 HSP 7-Nov-6 Dark Chocolate 40 ml vial + vac(30sec) + 5hr 5C 60 C for 5 min. Splitless DB 5m length x 0.5mm ID, 0.5µm film DB 30m length x 0.5mm ID, 0.5µm film He,.5cc/min. constant flow 40 C hold 5min., 0 C/min. to 35C, 35 hold 5min. (solvent 6min) Agilent 7890B/5977A amu,.8 scans/sec Propanoic acid, -methyl-. Butanoic acid, 3-methyl- 3. Butanoic acid, -methyl- 4. Heptanal 5. Pyrazine,,5-dimethyl- 6. Benzaldehyde 7. Pentanoic acid, 4-methyl- 8. Hexanoic acid 9. Pyrazine, trimethyl- 0. Propanoic acid, -hydroxy-, butyl ester. D-Limonene. Ethanone, -(H-pyrrol--yl)- 3. Acetophenone 4. Pyrazine, 3-ethyl-,5-dimethyl- 5. Pyrazine, tetramethyl- 6. -Nonanone 7. Nonanal 8.,6-Octadien-3-ol, 3,7-dimethyl- 9. Octanoic acid, ethyl ester 0. Benzeneacetic acid, ethyl ester. Acetic acid, -phenylethyl ester. Benzeneacetaldehyde,.alpha.-ethylidene- 3. Vanillin 4. Benzoic acid, pent--yl ester 5. Tetradecane 6. 5-Methyl--phenyl--hexenal 7. Pentadecane 8. Butylated Hydroxytoluene 9. H--Benzopyran--one, 3,4-dihydro-8-hydroxy-3-methyl- 30. Dodecanoic acid, ethyl ester 3. Benzophenone 3. Tetradecanoic acid, ethyl ester 33 Caffeine 34. -Heptadecanone 35. Hexadecanoic acid, methyl ester 36. Di-sec-butyl phthalate Octadecenoic acid, methyl ester 38. Linoleic acid ethyl ester Octadecenoic acid, (E)- 40. Octadecanoic acid, ethyl ester 9

Coffee Analysis 9.5e+08.4e+08.3e+08.e+08.e+08 4 8 e+08 6 4 9e+07 8e+07 7e+07 7 6e+07 5 8 5e+07 0 3 4e+07 3e+07 e+07 e+07 3 5 6 7 8 9 0 3 4 7 3 5 6 9 30 0.00 5.00 0.00 5.00 30.00 35.

Breakroom coffee 0 ml vial + vac(30sec) + 3hr equilibration @ 60C 60 C for 5 min. Splitless DB 5m length x 0.5mm ID, 0.5µm film DB 30m length x 0.5mm ID, 0.5µm film He,.5cc/min.

3-Furaldehyde 4. -Furanmethanol 5. Butyrolactone 6. Ethanone, -(-furanyl)- 7. Pyrazine,,5-dimethyl- 8. -Furancarboxaldehyde, 5-methyl- 9. Phenol 0. -Furanmethanol, acetate. H-Pyrrole--carboxaldehyde.

11 Coffee Analysis 9.5e+08.4e+08.3e+08.e+08.e e e+07 8e+07 7e e e e+07 3e+07 e+07 e Instrument: Run date: Sample description: Amount of sample (g): Sample conditions: Desorb conditions: Split Mode: Precolumn: Column: Carrier: Oven Temp: GCMS: MS Operation: Pen ID: 5800HSP 8-Nov-6 Breakroom coffee 0 ml vial + vac(30sec) + 3hr 60C 60 C for 5 min. Splitless DB 5m length x 0.5mm ID, 0.5µm film DB 30m length x 0.5mm ID, 0.5µm film He,.5cc/min. constant flow 40 C hold 5min., 0 C/min. to 35C, 35 hold 5min. (solvent 6min) Agilent 7890B/5977A amu,.8 scans/sec Pyridine. 3(H)-Furanone, dihydro--methyl Furaldehyde 4. -Furanmethanol 5. Butyrolactone 6. Ethanone, -(-furanyl)- 7. Pyrazine,,5-dimethyl- 8. -Furancarboxaldehyde, 5-methyl- 9. Phenol 0. -Furanmethanol, acetate. H-Pyrrole--carboxaldehyde. Ethanone, -(H-pyrrol--yl)- 3. Ethanone, -(-methyl-h-pyrrol--yl)- 4. Phenol, -methoxy- 5. H-Pyrrole, -(-furanylmethyl)- 6. Phenol, 4-ethyl--methoxy- 7. Indole 8. Furan,,'-[oxybis(methylene)]bis- 9. -Methoxy-4-vinylphenol 0. Benzene, 4-ethenyl-,-dimethoxy-. H-Pyrrole, -(-furanylmethyl)-. Phenol,,5-bis(,-dimethylethyl)- 3. Dodecanoic acid, ethyl ester 4. Caffeine 5. -Hexadecanol 6. Hexadecanoic acid, methyl ester 7. n-hexadecanoic acid 8. Isopropyl palmitate 9. Octadecanoic acid 30. Hexadecanamide 3. 9-Octadecenamide, (Z)- Cashew Analysis.e+08 3.e+08 e+08 9e+07 8e+07 7e+07 6e+07 5e+07 4e+07 3e+07 e+07 e+07 Instrument: Run date: Sample description: Amount of sample (g): Sample conditions: Desorb conditions: Split Mode: Precolumn: Column: Carrier: Oven Temp: GCMS: MS Operation: Pen ID: HSP -Nov-6 Cashews 40 ml vial + vac(30sec) + 48hr 5C 60 C for 5 min. Splitless DB 5m length x 0.5mm ID, 0.5µm film DB 30m length x 0.5mm ID, 0.5µm film He,.5cc/min. constant flow 40 C hold 5min., 0 C/min. to 35C, 35 hold 5min. (solvent 6min) Agilent 7890B/5977A amu,.8 scans/sec H-Pyrrole, -methyl-. Toluene 3 Hexanal 4. Ethylbenzene 5. o-xylene 6. Bicyclo[4..0]octa-,3,5-triene 7. Pyrazine,,5-dimethyl- 8. Benzaldehyde 9. Benzeneacetaldehyde 0. D-Limonene. Nonanal. 4H-Pyran-4-one,,3-dihydro-3,5-dihydroxy-6-methyl- 3. Dodecane 4. -Methoxy-4-vinylphenol 3 5.,4-Decadienal, (E,E)- 6. Tridecane, 5-methyl Copaene 8. Tetradecane 9. Caryophyllene 0. Humulene. Aromandendrene. Pentadecane 3. Butylated Hydroxytoluene 4..beta.-Bisabolene 5. Hexadecane 6. Octadecane 7. Benzene, (-methylundecyl)- 8. Dibutyl phthalate 9. n-hexadecanoic acid 30. Isopropyl palmitate 3. 9-Octadecenoic acid, methyl ester, (E)- 3. Diisooctyl phthalate

12 3 Rum Analysis.6e+08.4e+08.e+08 e+08.8e+08.6e+08.4e+08.e+08 e+08 8e+07 6e+07 4e+07 e e e+07.3e+07.e+07 4.e+07 e Instrument: Run date: Sample description: Amount of sample (ml): Sample conditions: Desorb conditions: Split Mode: Precolumn: Column: Carrier: Oven Temp: GCMS: MS Operation: Pen ID: 5800 HSP 6-Nov-6 : Rum (50µl BB + 50µl Water) 50µl 0mL vial + vac(30sec) + 5hr 5 C 60 C for 5 min. Splitless DB 5m length x 0.5mm ID, 0.5µm film DB 30m length x 0.5mm ID, 0.5µm film He,.5cc/min. constant flow 40 C hold 5min., 0 C/min. to 300 C, hold 7min. (solvent 8min) Agilent 7890B/5977A amu,.8 scans/sec (H)-Furanone, dihydro--methyl-. -Hexanol 3. Ethanone, -(-furanyl)- 4. Hexanoic acid, ethyl ester 5. Pentanoic acid, 4-oxo-, ethyl ester 6. Phenylethyl Alcohol 7. Butanedioic acid, diethyl ester 8. Octanoic acid, ethyl ester 9. trans-3-methyl-4-octanolide 0. n-decanoic acid. Decanoic acid, ethyl ester. Octanoic acid, 3-methylbutyl ester 3. Dodecanoic acid 4. Benzoic acid, 4-hydroxy-3-methoxy-, ethyl ester 5. Dodecanoic acid, ethyl ester 6. Pentanoic acid,,,4-trimethyl-3-carboxyisopropyl, isobutyl ester 7. Benzophenone 8. Pentadecanoic acid, 3-methylbutyl ester 9. Tetradecanoic acid 0. Ethyl 9-tetradecenoate. Pentadecanoic acid, ethyl ester. Isopropyl myristate 3. -Hexadecanol 4. Pentadecanoic acid, 4-methyl-, methyl ester 5. n-hexadecanoic acid 6. Ethyl 9-hexadecenoate 7. Hexadecanoic acid, ethyl ester 8. -Tetradecyl acetate 9. Isopropyl palmitate Octadecenoic acid (Z)-, methyl ester 3. Heneicosane 3. Methyl stearate 33. Ethyl 9-hexadecenoate 34. Octadecanoic acid, ethyl ester 35. Benzoic acid, tridecyl ester

13 Analysis of Odor Producing Compounds to Less Than Part Per Trillion Using Vacuum Extraction Evacuation (30 seconds) Desorb Gas Port Micro Seal for Evacuation Silonite coated 36 Stainless Steel Sample extracts much faster at 30x below atmospheric pressure, limited by vapor pressure of water at 5 C 60mg Tenax TA Figure (below) Sorbent Pens containing 60mg of Tenax perform vacuum extraction on 50mL of sample at 5 C for to 0 hours, followed by direct, splitless desorption into a GCMS. The tops of the Sorbent Pens were heated to 50 C to prevent water condensation. Sampled Sorbent 5m, 50um ID, 0.5um DB Vacuum Extraction of water & wine using Sorbent Pens. Vacuum remains even after removal of vacuum source 60m, 50um ID, 0.5um DB Clean Sorbent Pens 5800 Sorbent Pen Desorption Unit on GCMS

14 Sorbent Pen Vacuum Extraction of Odors Kinetics Study Comparing Recoveries of a 0 PPt Standard in Water After, 3, 8, 6 Hour Extraction Times Extractions performed without salting to prevent adsorbent damage via aerosol transport Temp = 5 C. Sorbent Pens heated to 30 C to prevent water condensation An overnight extraction appears to bring the Pens to near equilibrium with the sample hour 3 hour 8 hour 6 hour -Methylisoborneal Instrument: Run date: Sample description: 5800 HSP 5//6 Geosmin and Halonanisoles spiked into 50mL filtered water Concentration of sample: 0ng/L Sample conditions: 5mL vial + vac + 00rpm agitation + {,,3,8,6} hours at 5 C Split Mode: Splitless Desorb Conditions: 5min at 60 C Pre-column: DB 5m length x 0.5mm ID, 0.5 µm film thickness Column: DB 60m length x 0.5mm ID, 0.5 µm film thickness Carrier: He,.5mL/min constant flow Oven Temp: 35 C, 0 C/min. to 80 C, hold 4min. GCMS: Agilent 7890B/5977A MS Operation: amu,.5 scans/sec hour 3 hour Geosmin 8 hour 6 hour Figures,3 (above) Relative responses for target compounds extracted from 0ng/L standards in 50cc filtered water at 5 C, no salt added, 00 rpm agitation, /30th atm vacuum, for,3,8, and 6 hours. A final extraction time of 0 hours was selected for this method with an extraction efficiency between 60-80%. 3

15 Sorbent Pen Kinetic Study Instrument: Run date: Sample description: 5800 HSP 5//6 Geosmin and Halonanisoles spiked into 50mL filtered water Concentration of sample: 0ng/L Sample conditions: 5mL vial + vac + 00rpm agitation + {,,3,8,6} hours at 5 C Split Mode: Splitless Desorb Conditions: 5min at 60 C Pre-column: DB 5m length x 0.5mm ID, 0.5 µm film thickness Column: DB 60m length x 0.5mm ID, 0.5 µm film thickness Carrier: He,.5mL/min constant flow Oven Temp: 35 C, 0 C/min. to 80 C, hold 4min. GCMS: Agilent 7890B/5977A MS Operation: amu,.5 scans/sec.. 3.,4,6-Trichloroanisole,3,5-Trichloroanisole,3,4-Trichloroanisole hour 3 hour 8 hour 6 hour hour 3 hour 8 hour 6 hour,4,6-tribromoanisole Figures 4,5 (above) Relative responses for target compounds extracted from 0ng/L standards in 50cc filtered water at 5 C, no salt added, 00 rpm agitation, /30th atm vacuum, for,3,8, and 6 hours. A final extraction time of 0 hours was selected for this method with an extraction efficiency between 60-80%. 4

16 Sorbent Pens A revolutionary extraction technology that is quantitative by design. Entech Instruments 07 Agate Court Simi Valley, CA Phone: Learn more online Visit us at entechinst.com Sorbent Pens Entech Instruments 07. Sorbent Pen, MicroValve, Silonite, Micro-QT, MiniCan, and Bottle-Vac, are trademarks of Entech Instruments. All Rights Reserved.

Sorbent Pen Heavy & Labile SVOC s Taints, Off-Flavors, Odors

Revolutionary extraction technology quantitative by design. Say Goodbye to SPME... and hello to Sorbent Pens! A revolutionary new extraction technology. Sorbent Pen Heavy & Labile SVOC s Taints, Off-Flavors,