spme-ffa field sampler (ffa-fs)

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CHROMLINE

Via Anita Garibaldi,40 59100 Prato (PO) – Italy

Phone: +39 335 1890076 Fax: +39 0574 660136 Email: [email protected] web: www.chromlinesrl.com

©2010 CHROMLINE SRL. Printed in Italy. Version 1.4

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Manual

SPME-FFA Field Sampler

Chromline Srl Via Anita Garibaldi, 40

59100 Prato (PO) Italy

Phone: +39 335 1890076 FAX: +39 0574 660136

email: [email protected] web: www.chromlinesrl.com

Cat.No. 57554-U

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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.

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

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

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REPLACEMENT PARTS & ACCESSORIES

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

FFA57293-U PK3, 65μm PDMS-DVB Stableflex SPME Fast Fit Assembly 23ga

FFA57327-U PK3, 65 μm PDMS-DVB Stableflex SPME Fast Fit Assembly 24 ga

FFA57298-U PK3, 50/30 μm DVB/CAR/PDMS Stableflex SPME Fast Fit Assembly 23 ga

FFA57329-U PK3, 50/30 μm DVB/CAR/PDMS Stableflex SPME Fast Fit Assembly 24 ga

FFA57341-U PK3, 100 μm PDMS SPME Fast Fit Assembly 23 ga

FFA57301 PK3, 100 μm PDMS SPME Fast Fit Assembly 24 ga

FFA57294-U PK3, 85 μm POLYACRYLATE SPME Fast Fit Assembly 23 ga

FFA57305 PK3, 85 μm POLYACRYLATE SPME Fast Fit Assembly 24 ga

FFA57295-U PK3, 85 μm CAR/PDMS STABLEF. SPME Fast Fit Assembly 23 ga

FFA57335-U PK3, 85 μm CAR/PDMS STABLEF. SPME Fast Fit Assembly 24 ga

FFA57354-U PK3, 60 μm PEG Metal SPME Fast Fit Assembly 23 ga





FFA Fibers

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RECOVERY OF INNER PLUNGER In case the inner plunger gets accidentally pushed in without having the external plunger properly in-stalled, 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

TROUBLE SHOOTING

STATION FOR NEEDLE PROTECTOR REMOVAL (57583-U) When the needle protector of the FFA-FS has gotten contaminated it can be re-moved 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 sam-ple without touching the contaminated part.

H1

H2

Fig. 32 - Station for needle protector removal.

Fig. 33 - Double plain face of needle protec-tor as seat for wrench or removal station

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SPME-FFA Field Sampler (FFA-FS) The SPME-FFA Field Sampler (FFA-FS) is de-signed 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 incor-porates 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 sam-pler 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. Alter-natively the FFA can be removed from the field sampler and be placed in an option-al 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 au-tosampler. The MFX system is available as 3-Pos. and 25-Pos. System (45-Pos. as custom). Please see also page 11 in this manual.

* available from Gerstel GmbH & Co KG

References: Anal. Chem 2000, 72, 5178-5186 Koziel, J.; Jia, M.; Pawliszyn, J. Air Sampling with Porous Solid Phase Microextraction Fibers

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FIELD SAMPLER PARTS

Fig. 1 - FFA-Field Sampler(FS) Parts

Fig. 3 - Needle Septa 5x3 mm (Cat.# 57571-U).

Fig. 4 - for 23ga beveled tip fibers — no identification notch (Cat# 57557-U).

Fig. 5 - for 23ga blunt tip fibers — one identification notch (Cat# 57562-U).

Fig. 6 - for 24ga blunt tip fibers — two identification notches (Cat# 57561-U).

Fig. 7 - Stainless steel Needle Guide. (Cat# 57556-U).

PTFE Sealing Cups & Needle Guide

Fig. 2 – Plunger recovery tool. (Cat.# 57529-U).

B1

B2

B3

Plunger Cap(Part A1)

(RSS010)

Sealing Assembly/Unit with Plunger Cap (Part A)

(RSS000B)

PTFE Sealing Cups (Part B)

SS Needle Guide (Part C)

Septa Nut (Part E) (RSS005)

Needle Septa

Manual Desorption Adapter

(Optional Accessory)

Plunger Recovery Tool

Sampler Body Screw (Part F) (RSS004)

Needle Protector (RSS000C)

Plunger (RSS003)

Sampler Body

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Name

Conc. (mg/m3) in

Tedlar bag 25 L

% Loss after 15 days @

-4 °C

RSD%

(n=5)


Room Temp.(+20-

25 °C)

RSD%

(n=5)


+40 °C

RSD%

(n=5)

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

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

Optional FFA Storage

After sampling, the FFA can also removed from the field sampler and be stored in an optional FFA Storage Con-tainer (57592-U). This storage container is employing the same PTFE sealing mechanism.

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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 men-tioned in below table. For details on this study please contact Chromline under [email protected].

Fig. 38 - Fiber after conditioning.

Fig. 39 - Fiber after15 days sealed by Chromline PTFE sealing cup.

PTFE SEALING UP DATA

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ACCESSORIES

Fig. 8 - FFA-FS manual desorption adapt-er (Cat.# 57568-U).

SPME-FFA to be used in this Field Sampler 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. 10 - SPME-FFA.

Fig. 9 - Optional station for convenient Needle Protector removal (Cat.# 57583-U).

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PTFE SEALING CUP INSTALLATION

Fig. 11 - Open FS plunger assembly by unscrewing the sealing assembly (Part A)

Fig. 12 - Sealing assembly out of plunger (Part A).

Part A

Fig. 13 - Chose PTFE cap (Part B1, B2, B3) according to SPME needle being used. See page 5 for details.

Part B1 23ga bev.

Part B2 23ga bl.

Part B3 24ga bl.

Part C

Fig. 14 - Assemble parts A,B (B1, B2 or B3) and C.

Fig. 15 - Re-install Part A into the plunger assembly

Data on PTFE sealing efficiency can be found in the Appendix.

Part A

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AUTOMATIC DESORPTION WITH MFX

Fig. 33 – For automated desorption open FFA-FS to remove FFA.

Fig. 34 - Place the FFA fiber in MFX tray.

Fig. 35 - SPME Fiber Saver on the MFX tray keep the fibers sealed befo-re 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:

www.gerstel.com/en/multi-spme-fiber-exchange-mfx.htm

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MANUAL DESORPTION 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

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.

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 pro-tection like shown in Fig. 28.

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.

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Fig. 16 - Unscrew Septa Nut (Part E). Fig. 17 - Insert silicone septa into part E and re-install part E on the sampler

Part E

Part E

INSTALLATION OF NEEDLE SEPTA

FFA INSTALLATION

Fig. 18 - FFA fiber. 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.

Fig. 20 - Re-assemble and tighten the FS. In this status the sampler can be transported to the sampling site main-taining the conditioning of the FFA.

Part F

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SAMPLING

Fig. 21 - Remove plunger from holder (1). Detach plunger cap (Part A1) from the plunger by unscrewing it.

Fig. 23 - Insert flat point of plunger in pos.1 and slide to pos. 2 to lock.

Fig. 24 - For sampling, press the plunger until you hear/feel a click.

Fig. 25 - The fiber is now exposed within the needle protector cage for sampling

Fig. 26 - To retract the fiber after sam-pling proceed in revese order (Fig.24 to 21. Pull the plunger and remove it .

Fig. 22 - Insert plunger cap into the opening on the other end of the plung-er for storage.

2 1

Part A1

Part A1

1

2

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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

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 re-tracting the fiber. In case the sampling was done in a contaminated area, one can clean the device, e.g. with sodium hypo-chlorite solution. Testing by storing the sampler for 15 days in sodium hypo-chlorite 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. 29 - FFA-FS closed and ready for cleaning procedure.

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)

spme-ffa field sampler (ffa-fs)

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