SPME-FFA Field Sampler

Page 16 SPME-FFA Field Sampler Manual Page 1 Cat.No. 57554-U CHROMLINE Via Anita Garibaldi,40 59100 Prato (PO) Italy Phone: +39 335 1890076 Fax: +39 0574 660136 Email: info@chromlinesrl.com web: www.chromlinesrl.com 2010 CHROMLINE SRL. Printed in Italy. Version 1.4 Chromline Srl Via Anita Garibaldi, 40 59100 Prato (PO) Italy Phone: +39 335 1890076 FAX: +39 0574 660136 email: info@chromlinesrl.com web: www.chromlinesrl.com

Page 2 Page 15 REPLACEMENT PARTS & ACCESSORIES IMPORTANT NOTE This holder accepts only SPME Fast Fit Assemblies (FFA). Standard SPME ibers do not work and can be damaged when attempted to be used with this holder. Products included with 57554-U: 1x SPME-FFA Field Sampler 1x Plunger Recovery Tool 1x Needle Septa 5x3mm 1x Stainless Steel Needle Guide 1x PTFE Sealing Cup 23ga Blunt Tip Fibers one notch 1x PTFE Sealing Cup 24ga Blunt Tip Fibers two notches 1x PTFE Sealing Cup 23ga Bevel Tip fibers no notch FFA Fibers FFA57293-U FFA57327-U FFA57298-U FFA57329-U FFA57341-U FFA57301 FFA57294-U FFA57305 FFA57295-U FFA57335-U FFA57354-U FFA57309 FFA57302 FFA57289-U FFA57291-U PK3, 65μm PDMS-DVB Stableflex SPME Fast Fit Assembly 23ga PK3, 65 μm PDMS-DVB Stableflex SPME Fast Fit Assembly 24 ga PK3, 50/30 μm DVB/CAR/PDMS Stableflex SPME Fast Fit Assembly 23 ga PK3, 50/30 μm DVB/CAR/PDMS Stableflex SPME Fast Fit Assembly 24 ga PK3, 100 μm PDMS SPME Fast Fit Assembly 23 ga PK3, 100 μm PDMS SPME Fast Fit Assembly 24 ga PK3, 85 μm POLYACRYLATE SPME Fast Fit Assembly 23 ga PK3, 85 μm POLYACRYLATE SPME Fast Fit Assembly 24 ga PK3, 85 μm CAR/PDMS STABLEF. SPME Fast Fit Assembly 23 ga PK3, 85 μm CAR/PDMS STABLEF. SPME Fast Fit Assembly 24 ga PK3, 60 μm PEG Metal SPME Fast Fit Assembly 23 ga PK3, 30 μm PDMS SPME Fast Fit Assembly 24 ga PK3, 7 μm PDMS SPME Fast Fit Assembly 24 ga PK3, 30 μm PDMS SPME Fast Fit Assembly 23 ga PK3, 7 μm PDMS SPME Fast Fit Assembly 23 ga INDEX INTRODUCTION 3 SPME-FFA FIELD SAMPLER PARTS 4 ACCESSORIES 5 INSTALLATION OF PTFE SEALING CUP, SEPTA, AND FFA 6 SAMPLING 8 CLEANING OF FIELD SAMPLER 9 DESORPTION MANUAL & AUTOMATED BY MFX 10 APPENDIX PTFE SEALING DATA 12 TROUBLE SHOOTING RECOVERY OF INNER PLUNGER 14 REPLACEMENT PARTS 15 PTFE Sealing System & Septa 57557-U PK3, PTFE sealing cups 23ga beveled no identification line (SFSC23BE) 57562-U PK3, PTFE sealing cups 23ga blunt one identification line (SFSC23BL) 57561-U PK3, PTFE sealing cups 24ga blunt two identification lines (SFSC24BL) 57571-U Needle Septa, Pk3. (RSS000E) Replacement Parts 57556-U Stainless steel needle guide (SFSC000A) 57574-U FFA-FS O-ring kit (RSS000D) 57564-U FFA-FS Needle protector (RSS000C) 57565-U FFA-FS Sampler body screw (RSS004) 57593-U FFA-FS Needle septa nut (RSS005) 57555-U FFA-FS Sealing mechanism with plunger end cap (RSS000B) 57528-U FFA-FS Plunger cap (RSS010) Accessories 57568-U FFA-FS manual desorption adapter (RSS000F) 57529-U Plunger Recovery Tool (RSS000H) 57583-U Station for Needle Protector Removal (RSS000G) 57592-U SPME FFA Storage Container

TROUBLE SHOOTING Page 14 SPME-FFA Field Sampler (FFA-FS) Page 3 RECOVERY OF INNER PLUNGER In case the inner plunger gets accidentally pushed in without having the external plunger properly installed, the enclosed plunger recovery tool can be used to pull the inner plunger Fig. 29 Inner plunger accidentially pressed in Fig. 30 Plunger recovery tool. Fig. 31 Insert the tool to retrieve the inner plunger STATION FOR NEEDLE PROTECTOR REMOVAL (57583-U) When the needle protector of the FFA-FS has gotten contaminated it can be removed by using the Needle Protector Removal Station. Affix the station e.g. on table or on an instrument using the screw holes H1 and H2 (screws not included). Insert the needle into the station and unscrew the part. Now you can inject the sample without touching the contaminated part. The SPME-FFA Field Sampler (FFA-FS) is designed to be used with SPME Fast Fit fiber Assemblies (FFAs). It is suitable for various kinds of field sampling applications by exposing the installed fiber to the environment to be sampled. The sampler is selfcontained and allows safe storage of a conditioned or sampled SPME fiber (only SPME FFA). The plunger assembly in this holder works as an actuator to expose the fiber but also incorporates a sealing mechanism to safely transport the conditioned or sampled fiber from and/or to the laboratory. This allows the user to prepare and set up the sampler in a clean environment (e.g. laboratory). At the sampling site the user just needs to remove the plunger/protection and expose the fiber to the environment. Only the needle part of the SPME FFA gets into contact with the sampled environment. The rest of the FFA stays sealed off in the holder until removal from the sampler. After sampling the plunger with its sealing mechanism/ protection serves to safely store and transport the sampled fiber until analysis. Alternatively the FFA can be removed from the field sampler and be placed in an optional SPME FFA Storage Container (Cat.No. 57592-U). Desorption of the sampled FFA into the GC instrument can be done manually with the FFA-FS using an optional desorption adapter (Cat.#57568-U) or by placing the FFA into a Multi Fiber Exchanger System (MFX)* suitable for CTC Combipal Type autosampler. The MFX system is available as 3-Pos. and 25-Pos. System (45-Pos. as custom). Please see also page 11 in this manual. H2 H1 Fig. 32 - Station for needle protector removal. Fig. 33 - Double plain face of needle protector as seat for wrench or removal station References: Anal. Chem 2000, 72, 5178-5186 Koziel, J.; Jia, M.; Pawliszyn, J. Air Sampling with Porous Solid Phase Microextraction Fibers * available from Gerstel GmbH & Co KG

Page 4 Page 13 FIELD SAMPLER PARTS Plunger Recovery Tool Manual Desorption Adapter (Optional Accessory) Sampler Body Screw (Part F) (RSS004) Needle Septa Sampler Body Name Conc. (mg/m 3 ) in Tedlar bag 25 L % Loss after 15 days @ -4 C RSD% (n=5) % Loss after 15 days @ Room Temp.(+20-25 C) RSD% (n=5) % Loss after 15 days @ +40 C Dichloromethane 16,625-6,9 6,6-4,6 7,9-11,3 8,2 MTBE 9,25-2,8 9,8-7,2 4,3-4,3 9,2 n-hexane 8,25-4,3 8,7-8,1 4,6-6,1 6,7 RSD% (n=5) PTFE Sealing Cups (Part B) Plunger Cap(Part A1) (RSS010) SS Needle Guide (Part C) Septa Nut (Part E) (RSS005) Needle Protector (RSS000C) Plunger (RSS003) Sealing Assembly/Unit with Plunger Cap (Part A) (RSS000B) 1,1,1 Trichloroethane 16,75-4,9 6,2-1,4 8,6-3,5 9,7 1,2 Dichloroethane 15,625-3,9 9,3-6,3 4,1-7,3 4,5 Benzene 11-5,3 4,1-6,7 4,1-5,5 6,2 Trichloroethylene 18,25-6,1 6,6-4,5 8,6-4,8 7,5 Toluene 10,875-4,7 6,8-7,8 6,5-6,3 2,9 Tetrachloroethylene 20,25-4,2 7,4-3,1 7,3-3,3 8,1 Ethylbenzene 10,875-5,5 5,3-5,7 4,5-6,1 5,0 m + p Xylene 10,75-5,1 3,7-4,0 7,5-4,9 5,5 o-xylene 11-4,8 6,1-6,8 4,6-6,2 3,5 1,3,5 Trimethylbenzene 10,875-3,5 8,8-4,3 5,5-5,9 5,4 1,2,4 Trimethylbenzene 10,875-5,6 6,3-5,1 4,5-5,5 8,3 Fig. 1 - FFA-Field Sampler(FS) Parts Fig. 2 Plunger recovery tool. (Cat.# 57529-U). Fig. 3 - Needle Septa 5x3 mm (Cat.# 57571-U). Optional FFA Storage PTFE Sealing Cups & Needle Guide B1 Fig. 4 - for 23ga beveled tip fibers no identification notch (Cat# 57557-U). B3 Fig. 6 - for 24ga blunt tip fibers two identification notches (Cat# 57561-U). After sampling, the FFA can also removed from the field sampler and be stored in an optional FFA Storage Container (57592-U). This storage container is employing the same PTFE sealing mechanism. B2 Fig. 5 - for 23ga blunt tip fibers one identification notch (Cat# 57562-U). Fig. 7 - Stainless steel Needle Guide. (Cat# 57556-U).

PTFE SEALING UP DATA Page 12 The Chromline sealing mechanism ensures integrity of fiber conditioning as well as enabling storage of the sampled fiber. Below chromatograms show a cleaned fiber immediately desorbed and after conditioning (Fig. 38) and after15 days sealed with the PTFE Sealing Cap used in the FFA-FS (Fig. 39). The sealed fibers were exposed to the atmosphere below mentioned compounds and concentrations. No contamination could be observed in that time. With the same test set up the storage stability of a sample was evaluated for the same mix of VOCs at different tempratures was evaluated. Temperatures was -4 C, room temperature (+20-25 C) and +40 C. The test was done with 85μm CAR/PDMS 23ga fiber (the same fibers were used for each temperature). For sampling the fibers were exposed 15 sec to the atmosphere of compounds mentioned in below table. For details on this study please contact Chromline under info@chromlinesrl.com. ACCESSORIES Fig. 8 - FFA-FS manual desorption adapter (Cat.# 57568-U). Page 5 Fig. 9 - Optional station for convenient Needle Protector removal (Cat.# 57583-U). SPME-FFA to be used in this Field Sampler Fig. 38 - Fiber after conditioning. Fig. 10 - SPME-FFA. The SPME Fast Fit Assemblies (FFA) are a configuration of SPME fibers allowing the automated exchange of SPME fibers by the Multi Fiber EXchange (MFX) system on an autosampler. For the most recent listing of products, please refer to sigma-aldrich.com/spme FFA Barcode Labeling Provides the user and the autosampler with information about the properties of the SPME fast fit fiber assembly: A. The color code indicates the phase type. The coding is the same as for the colored screw hub of the traditional SPME fiber assemblies B. The first 2 digits of the barcode identify the fiber type, incorporating the phase and the gauge size. C. The remaining digits represent a unique tracking number for sample traceability. Fig. 39 - Fiber after15 days sealed by Chromline PTFE sealing cup.

Page 6 Page 11 PTFE SEALING CUP INSTALLATION AUTOMATIC DESORPTION WITH MFX Part A Part A Fig. 11 - Open FS plunger assembly by unscrewing the sealing assembly (Part A) Fig. 12 - Sealing assembly out of plunger (Part A). Fig. 33 For automated desorption open FFA-FS to remove FFA. Fig. 34 - Place the FFA fiber in MFX tray. Part B1 23ga bev. Part B2 23ga bl. Part B3 24ga bl. Part C Fig. 13 - Chose PTFE cap (Part B1, B2, B3) according to SPME needle being used. See page 5 for details. Fig. 14 - Assemble parts A,B (B1, B2 or B3) and C. Fig. 15 - Re-install Part A into the plunger assembly Fig. 35 - SPME Fiber Saver on the MFX tray keep the fibers sealed before being analyzed. Fig. 36 - MFX tray with 25 FFA positions. A MFX with 3 positions is available and as custom one with 45 positions Fig. 37 - Example set up: GERSTEL MPS autosampler with MFX 3-Position option on Agilent Technologies GC7890+ MSD. MFX System For more information on the Multi Fiber EXchanger System please refer to the Gerstel website: Data on PTFE sealing efficiency can be found in the Appendix. www.gerstel.com/en/multi-spme-fiberexchange-mfx.htm

MANUAL DESORPTION Page 10 INSTALLATION OF NEEDLE SEPTA Page 7 By installing the manual desorption adapter for the FS (Cat.# 57568-U) sampled fibers can directly be inserted into a GC injector block for desorption. Remove plunger and install as described in Fig. 21-23 Part E Fig. 30 - Remove the needle protection by unscrewing it from the sampler and attach the manual desorption adapter to the FS as indicated below. Install the plunger as described in Fig 23. Part E Fig. 16 - Unscrew Septa Nut (Part E). Fig. 17 - Insert silicone septa into part E and re-install part E on the sampler FFA INSTALLATION Fig. 31 - Inject the FFA needle into the GC injector port in a way that the adapter sits on the injector s septa screw. Make sure that the sampler does not tilt to prevent any needle bending. Push the plunger down to expose the fiber in the injector. The fiber is now getting desorbed. Fig. 32 - After desorption retract the fiber into the needle by pulling the plunger back, then remove the sampler from the injector port. To ensure the fiber does not get contaminated place the plunger back over the needle protection like shown in Fig. 28. Fig. 18 - FFA fiber. Part F Fig. 19 - Take FS apart by unscrewing the sampler body screw (Part F) as indicated and place FFA into the left hand part first. Use gentle force to push the FFA needle through the septa. Optional pre-pierce the septa with a syringe needle. Note: Please refer to your GC instrument manual for the distance of the injector top to the hottest part of the injector block. The Manual desorption adapter (Cat.No. 57568-U) is designed for an injection depth of 5 cm. Fig. 20 - Re-assemble and tighten the FS. In this status the sampler can be transported to the sampling site maintaining the conditioning of the FFA.

SAMPLING Page 8 Page 9 Part A1 2 Part A1 1 Fig. 21 - Remove plunger from holder (1). Detach plunger cap (Part A1) from the plunger by unscrewing it. 2 1 Fig. 23 - Insert flat point of plunger in pos.1 and slide to pos. 2 to lock. Fig. 22 - Insert plunger cap into the opening on the other end of the plunger for storage. Fig. 24 - For sampling, press the plunger until you hear/feel a click. Fig. 27 - Place the plunger back over the fiber protection for sealing. Fig. 28 - The FS can now be stored until analysis. After sampling in contaminated environments it might be advisable to clean the sampler before further handling. CLEANING PROCEDURE Fig. 29 - FFA-FS closed and ready for cleaning procedure. During sampling and when the sampler is closed, the inside part of the device is sealed off from the external environment. When the fiber is exposed, the movement of the plunger compresses the air inside the holder. There is no venting to the out side. By this, the interior of the sampler does not become contaminated when retracting the fiber. In case the sampling was done in a contaminated area, one can clean the device, e.g. with sodium hypochlorite solution. Testing by storing the sampler for 15 days in sodium hypochlorite solution showed no detrimental or negative effect on the integrity of the sampler. This test demonstrated the suitability of the sampler for use under extreme conditions. Fig. 25 - The fiber is now exposed within the needle protector cage for sampling Fig. 26 - To retract the fiber after sampling proceed in revese order (Fig.24 to 21. Pull the plunger and remove it. Optional FFA Storage After sampling, the FFA can also removed from the field sampler and be stored in an optional SPME-FFA Storage Container (57592-U)