ASPEC Positive Pressure Manifold. User's Guide

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Transcription:

ASPEC Positive Pressure Manifold User's Guide

This Page Is Intentionally Left Blank

Gilson, Inc. All rights reserved. All product and/or company names are trademarks of their respective holders. Use of the trademark(s) in this document does not imply any affiliation with or endorsements by the trademark holder(s).

CONTENTS CONTENTS Safety 6 Symbols, Signs, and Notices 6 Chemical Hazards 7 Flammable Solvents 7 Replacement Parts 7 Signs of Damage 7 Site Requirements 7 Storage and Movement 7 Sécurité 8 Symboles et Notes 8 Risques Chimiques 9 Solvants Inflammables 9 Pièces de Remplacement 9 Signes de Détérioration 9 Exigences du Site 9 Stockage et Déplacement 9 Introduction 10 Description 10 Technical Specifications 19 Setup 20 Set up or Replace the Manifold 20 Connect the Gas Supply 21 4 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Operation 22 Setup for Flow to Waste 22 Setup for Flow to Collection 23 Seat the Manifold 24 Unseat the Manifold 24 Control the Flow 25 General Flow Guidelines 27 Basic SPE Technique 28 Maintenance 31 Clean the ASPEC PPM 31 Install or Replace the O-Ring 31 Replace the Manifold Gasket 31 Maintenance Parts 31 Troubleshooting Table 32 Repair and Return Policies 36 Before Calling Us 36 Warranty Repair 36 Non-Warranty Repair 36 Return Procedure 37 Unit End-of-Life 37 Replacement Parts and Accessories 38 Configuration Kits 39 ASPEC Positive Pressure Unit 39 CONTENTS ASPEC Positive Pressure Manifold User's Guide 5

Safety Safety Read this section before installing and operating the instrument. Only trained technical personnel in a laboratory environment may use the instrument for non-medical, liquid handling purposes. For safe and correct use of the instrument, operating and service personnel must follow all instructions contained in this guide when installing, cleaning, and maintaining the instrument. All safety precautions must be observed during all phases of operation, service, and repair of the instrument. Failure to comply with these precautions or with warnings described in the user s guide violates safety standards of design, manufacture, and intended use of the instrument. Gilson assumes no liability for customers failing to comply with these requirements. Refer to the rear panel label on the instrument for the current standards to which the instrument has been found compliant. Read all documentation and safety information for accessories, peripherals, and other instruments that may be used with this instrument before operating the system. Symbols, Signs, and Notices Safety Notices The following safety notices may appear in this document: WARNING Indicates a potentially hazardous situation which, if not avoided, may result in personal injury. CAUTION Indicates a potentially hazardous situation which, if not avoided, may result in minor or moderate injury. NOTICE Indicates a potentially hazardous situation which, if not avoided, may result in equipment damage. 6 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Hazard Symbols The following hazard symbol may appear on the instrument or in this document: Symbol Explanation Explication Erläuterung Chemical Hazards Caution Attention Vorsicht Any chemicals used for analysis should be handled according to good laboratory practice (GLP). They should also be stored, used, and disposed of in accordance with the manufacturer s specifications, as well as local and national regulations. Potentially hazardous chemicals can be used with the instrument. Use care when handling chemicals and wear appropriate personal protective equipment (PPE), such as safety glasses, gloves, etc. The responsible individual must ensure that personnel are not exposed to hazardous levels of toxic substances as outlined in the material safety data sheets (MSDSs), or any documentation provided by local governing bodies such as The Health Protection Agency (United Kingdom) or The Occupational Safety and Health Administration (United States). Flammable Solvents Secure all flammable solvents. The temperature of liquids inside the system must be 25 C (77 F) below the lowest flame temperature of any solvents used. Replacement Parts Be sure to use only replacement parts mentioned in this user s guide. Refer to Replacement Parts and Accessories on page 38. Signs of Damage Do not attempt to use the instrument if there are visible signs of damage. Site Requirements Do not operate the instrument if site conditions are not within specifications. Refer to Technical Specifications on page 19 for more details. Storage and Movement Empty the drain well before moving the instrument. Safety ASPEC Positive Pressure Manifold User's Guide 7

Sécurité Sécurité Veuillez lire attentivement ce paragraphe avant toute installation ou utilisation de l instrument. Cet instrument est exclusivement destiné à être utilisé dans un environnement de laboratoire, par un personnel qualifié, à des fins de manipulations de liquides nonmédicales. Pour une utilisation correcte et en toute sécurité de l instrument, il est nécessaire que le personnel qui utilise et réalise la maintenance de l instrument, suive les instructions contenues dans ce guide lors de l installation, du nettoyage et de la maintenance de l instrument. Toutes les consignes de sécurité doivent être respectées durant toutes les phases de fonctionnement, d entretien ou de réparation de l instrument. Le non-respect de ces précautions ou des avertissements spécifiques mentionnés dans ce guide compromet les normes de sécurité de conception, de fabrication et d utilisation prévue de l instrument. Gilson décline toute responsabilité en cas d incapacité du client à se conformer à ces exigences. Merci de vous reporter aux indications mentionnées sur le panneau arrière de l instrument pour connaître les normes auxquelles l instrument a été déclaré conforme. Veuillez lire toute la documentation et les informations relatives à la sécurité pour les accessoires, périphériques, et autres instruments pouvant être utilisés avec cet instrument avant de faire fonctionner le système. Symboles et Notes Notes de Sécurité Les notes de sécurité suivantes peuvent apparaître dans ce document: AVERTISSEMENT Une situation potentiellement dangereuse qui, si elle n est pas évitée, peut entraîner des dommages corporels. ATTENTION Une situation potentiellement dangereuse qui, si elle n est pas évitée, peut entraîner des blessures mineures ou légères. AVIS Une situation potentiellement dangereuse qui, si elle n est pas évitée, peut entraîner des dommages matériels. 8 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Symbole de Dangers Le symbole de dangers suivants peuvent apparaître sur l instrument ou dans ce document: Symbol Explanation Explication Erläuterung Risques Chimiques Caution Attention Vorsicht Tous les produits chimiques utilisés pour l analyse doivent être manipulés conformément aux bonnes pratiques de laboratoire (BPL). Ils doivent être stockés, utilisés et éliminés conformément aux recommandations du fabricant ainsi qu aux réglementations locales et nationales. Manipuler les produits chimiques avec précaution et porter un équipement de protection individuelle adapté (EPI) comme des lunettes de sécurité, des gants, etc. Le responsable doit veiller à ce que le personnel ne soit pas exposé à des niveaux dangereux de substances toxiques comme indiqué dans les fiches de données de sécurité (fds), ou toute documentation fournie par les instances locales telles que l agence de protection de la santé (Royaume-Uni) ou l administration de la sécurité et de la Santé (Etats-Unis). Solvants Inflammables Prendre garde aux solvants inflammables. La température des solvants à l intérieur du système doit impérativement être inférieure de 25 C à la température de flamme la plus basse des solvants utilisés. Pièces de Remplacement Utiliser exclusivement les pièces détachées mentionnées dans ce guide utilisateur. Faire référence aux Replacement Parts and Accessories on page 38. Signes de Détérioration Ne pas utiliser le système en cas de signes de détérioration visibles. Exigences du Site Ne pas faire fonctionner l instrument si le site présente des conditions non conformes aux spécifications. Faire référence aux Technical Specifications on page 19. Stockage et Déplacement Vider le conteneur d evacuation des solvants usages avant de deplacer l appareil. Sécurité ASPEC Positive Pressure Manifold User's Guide 9

Introduction Introduction Description The ASPEC Positive Pressure Manifold provides uniform and consistent flow rate control for the cleanup of low or high viscosity samples, improves solid-phase extraction (SPE) reproducibility and recovery. The ASPEC PPM incorporates easily into laboratory workflows and provides a fast and simple way to prepare several samples for later analysis by chromatography. The ASPEC manifold offers a cost-effective approach to automation for environmental, clinical, forensic, and food or beverage testing laboratories. It is also an ideal choice for SPE cleanup prior to LCMS for bioanalyses. Safety Shield Protects users from solvents. Drain Well Refer to page 12 for a detailed description. SPE Racks 15-, 24-, and 96-positions available. SPE Collection Racks 15-, 24-, and 96-positions available. Manifold Locking Lever Forms the seal between the manifold and SPE cartridge when locked. Refer to page 14. Process Control Dial Switch between SPE and Dry controls to adjust gas flow. Refer to page 12 for more information. Pressure Gauge Monitors the operating pressure of the system, which should not exceed 15 psi. SPE Control Dial Switch between Low Flow and High Flow when the process control dial is set to SPE. Refer to page 12 for a detailed description. Figure 1 Standard Components of the ASPEC Positive Pressure Manifold (Left View) 10 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Manifold Retaining Clip Holds the manifold in place. Refer to page 20. Locator Plate Refer to page 14 for a detailed description. Thumbscrews Manifold Available in three configurations: 15- or 24-cartridge holders and 96-well plate holders. Manifold Positioning Lever Raises and lowers the manifold over the SPE cartridge holder. The manifold locking level must be unlocked to move this lever. Refer to page 14. Introduction Low Flow Adjustment Knob Used to fine tune flow when Low Flow is selected on the SPE control dial. Refer to page 13. Flow Adjustment Locks Used to lock in flow adjustments made with the low and high flow regulator knobs. Refer to page 13. High Flow Adjustment Knob Used to fine tune flow when High Flow is selected on the SPE control dial. Refer to page 13. Figure 2 Standard Components of the ASPEC Positive Pressure Manifold without Shield ASPEC Positive Pressure Manifold User's Guide 11

Introduction Control Dials Process Control Dial Used to select SPE (activates the SPE control dial to control high or low flow) or Dry (maximum flow). SPE Control Dial Used to select Low Flow, High Flow, or Off (to stop flow) when the process control dial is set to SPE. Drain Well Used primarily to flow the preparation solvents and matrix to waste. Ensure that the waste outlet tubing flows to a large waste container. Waste Outlet Tubing Rear Barbed Fitting Figure 3 Process Control Dial Figure 4 SPE Control Dial Figure 5 Collection and Drain Well with Waste Outlet Tubing Front Ejection Plate Used to quickly eject all the SPE cartridges from the cartridge rack. Slide the ejector plate through the standoffs on the SPE cartridge rack, and then push the plate up to eject the SPE cartridges. SPE Cartridges Standoffs Ejector Plate Figure 6 Ejecting SPE Cartridges 12 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Flow Adjustment Knobs Used to fine tune flow when Low Flow or High Flow is selected on the SPE control dial. Turn the adjustment knobs clockwise to open the valve and begin flow or to increase flow. Turn the adjustment knobs counterclockwise to decrease flow or to close the valve and stop flow. NOTE The loss of tension in the adjustment knobs indicates that the valve is fully closed. Flow Adjustment Locks Used to lock in flow adjustments made with the low and high flow adjustment knobs. Turn the flow adjustment locks clockwise to lock the low or high flow adjustment knobs. Turn the flow adjustment locks counterclockwise to unlock the low or high flow adjustment knobs. Introduction Flow Adjustment Locks High Flow Adjustment Knob Low Flow Adjustment Knob Figure 7 Low and High Flow Adjustment Knobs and Locks ASPEC Positive Pressure Manifold User's Guide 13

Introduction Locator Plate The front position of the locator plate is used as the active position, whereas the rear position accommodates the drain well when not in use. Manifold Locking Lever Forms the seal between the manifold and SPE cartridge holder when locked. Push the lever back to unlock (Red Lock Symbol, unlocked), and pull the lever forward to lock (Green Lock Symbol, locked). Manifold Positioning Lever Raises and lowers the manifold over the SPE cartridge holder. The manifold locking lever must be unlocked to move this lever. Push the lever back to lower the manifold (toward the Down position), and pull the lever forward to raise the manifold (toward the Up position). Rear (Unlocked) Front (Locked) Front Position Rear Position Figure 8 Locator Plate on the ASPEC PPM Front (Up) Rear (Down) Figure 10 Manifold Positioning Lever Figure 9 Manifold Locking Lever 14 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Pressure Gauge Monitors the operating pressure of the system, which should not exceed 15 psi. Figure 11 Pressure Gauge SPE Cartridge Plugs (Optional) Used to fill empty positions in the SPE cartridge racks (15- and 24-position). Introduction Plugs Rear Rows Empty Position SPE Cartridges (Front Row) Figure 12 Plugs on 24-Position Rack ASPEC Positive Pressure Manifold User's Guide 15

Introduction Unpacking The ASPEC Positive Pressure Manifold is delivered as a base unit (along with the safety shield) with one or more configuration kits for: 96 well SPE microplates (PN 37417014), 15-position SPE cartridge racks (6 ml, PN 37417013), and 24-position SPE cartridge racks (1 ml, PN 37417011 or 3 ml, PN 37417012). To safely remove the ASPEC PPM and accessories: 1. Open the top of the shipping container. 2. Remove the packing slip and bag containing the documentation, which will include: a printed user s guide, USB drive with video, items included checklist, and a quality control checklist. 3. Read the user s guide. 4. Remove the box containing the standard equipment and accessory kit, and then set it aside. 5. Check that all items specific to the configuration ordered and listed in Standard Equipment on page 17 are present. 6. Remove the safety shield nested in the foam, and then set it aside. 7. Grab the base of the ASPEC PPM firmly with two hands on opposing sides, and gently lift the ASPEC PPM out of the shipping box, and then set it on a laboratory bench that meets the site requirements on page 19. NOTE The ASPEC PPM ships and is nested within four molded foam pieces: two on the front and two on the back. Do not grip the ASPEC PPM by the manifold carrier or by the levers. 8. Hold the base of the ASPEC PPM, and then gently slide the molded foam pieces away from the base. 16 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Standard Equipment The following items are considered standard equipment and are provided with the ASPEC PPM. For part numbers, refer to Replacement Parts and Accessories on page 38. All Configurations Drain well (qty. 1) Gas supply tubing, 1/4" (OD), (qty. 1) Locator plate, dual position (qty. 1) O-ring manifold seal (qty. 1) Safety shield (qty. 1) Waste outlet tubing, Tygon 0.25" (OD), 3 ft. (qty. 1) Documentation ASPEC Positive Pressure Manifold User s Guide (qty. 1) USB drive with video of a sample protocol (qty. 1) Configuration Kit: 96-Position SPE Manifold Kit (PN 37417014) Gasket with adhesive-backed seal, 96-position (qty. 2) Manifold, SPE, 96-position (qty. 1) O-ring manifold seal (qty. 1) SPE plate adapter (qty. 1) 15-Position SPE Manifold Kit (6 ml, PN 37417013) Cartridge rack, SPE, 15-positions, 6 ml (qty. 1) Ejection plate for SPE cartridges (qty. 1) Gasket with adhesive-backed seal, 15-positions (qty. 2) Manifold, SPE, 15-positions (qty. 1) O-ring manifold seal (qty. 1) Tube rack for SPE collection, 6 ml (qty. 1) Introduction ASPEC Positive Pressure Manifold User's Guide 17

Introduction 24-Position SPE Manifold Kit (1 ml, PN 37417011) Cartridge ejection plate (qty. 1) Cartridge rack, SPE, 24-positions, 1 ml (qty. 1) Gasket with adhesive-backed seal, 24-positions (qty. 2) Manifold, SPE, 24-positions (qty. 1) O-ring manifold seal (qty. 1) Tube rack, SPE collection, 1 3 ml, 12 x 75 mm (qty. 1) 24-Position SPE Manifold Kit (3 ml, PN 37417012) Cartridge ejection plate (qty. 1) Cartridge rack, SPE, 24-positions, 3 ml (qty. 1) Gasket with adhesive-backed seal, 24-positions (qty. 2) Manifold, SPE, 24-positions (qty. 1) O-ring manifold seal (qty. 1) Tube rack, SPE collection, 1 3 ml, 12 x 75 mm (qty. 1) Recommended Accessories All Configurations Gas pressure regulator, 15 psi, external (qty. 1) 96-Position Microplate for SPE collection, 96-position, 1 ml (qty. 10) Microplate for SPE collection, 96-position, 2 ml (qty. 10) 15-Position Plugs to fill empty SPE cartridge spaces, 6 ml (qty. 15) Tubes, glass, collection, 10 ml, 15 x 85 mm (qty. 250) 24-Position Plugs to fill empty SPE cartridge spaces, 1 ml (qty. 24) Plugs to fill empty SPE cartridge spaces, 3 ml (qty. 24) Tubes, glass, collection, 5 ml, 12 x 17 mm (qty. 250) 18 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Technical Specifications Specification Dimensions (W x D x H) Liquid contact materials Site requirements Weight Description 33 x 48.3 x 44.2 cm (13 x 19 x 17.4 in.) Description Gasket Locator plate Specification Environment Inert gas supply 14.54 kg (32 lbs.) Material Neoprene Ertalyte Definition Indoor use only. If using volatile solvents, use a vent hood. Maximum pressure of 15 psi. Use 1/4" (OD) tubing. Introduction ASPEC Positive Pressure Manifold User's Guide 19

Setup Setup Set up or Replace the Manifold 1. Pull the manifold positioning lever forward (toward the Up position) until the manifold is fully raised. 2. Remove the manifold shield covering the manifold carrier, and then set it aside. 3. Turn (but do not remove) the thumbscrews counterclockwise to free the manifold retaining clip. Set the manifold retaining clip aside. 4. If necessary, remove the pre-installed manifold. NOTE Ensure that the O-ring does not fall out while removing the manifold. 5. Slide the new manifold into the manifold carrier with the orange O-ring on the back of the manifold facing the rear. 6. Reinstall the manifold retaining clip. 7. Turn the thumbscrews clockwise until finger tight. 8. Replace the manifold shield, and ensure that the standoff screws are seated properly on the manifold carrier. Manifold Shield Thumbscrews Manifold Carrier Manifold Manifold Retaining Clip Figure 13 Exploded View of Shield and Manifold Carrier 20 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Connect the Gas Supply 1. Locate the gas tubing supplied in the accessory kit. Connect the tubing from the rear quick connect port on the manifold to the quick connect port on the upper right side on the rear of the ASPEC PPM. Setup Plunger Insert Gas Tubing Figure 14 Gas Supply Connection (Rear View) Figure 15 Quick Connect Port with Tubing 2. Insert the gas wall supply tubing (1/4" OD, not provided) into the Gas Inlet quick connect port on the back of the instrument. NOTE The orange plunger insert will automatically engage the tubing. Pull back the tubing to check for proper engagement. Depress the orange plunger insert to release the tubing. NOTICE Ensure that the process control dial is set to Dry and the SPE control dial is set to Off before connecting the gas supply. Do not exceed 15 psi inlet pressure. 3. Use an external regulator to slowly increase pressure to the system up to 15 psi. 4. Switch the process control dial to SPE. ASPEC Positive Pressure Manifold User's Guide 21

Operation Operation Ensure that the following conditions are met before operating the ASPEC PPM: The SPE control dial is set to Off. The process control dial is set to SPE. The low and high flow adjustment knobs are closed. Refer to Flow Adjustment Knobs on page 13. The gas supply connection and regulator are properly installed. Refer to Connect the Gas Supply on page 21. Setup for Flow to Waste 1. Slide the locator plate to the front of the locator bed. 2. Place the drain well on the front position of the locator plate. 3. Connect the waste outlet tubing to the barbed fitting on the back of the collection and drain well. 4. Set the appropriate SPE cartridge rack with cartridges on the drain well. Waste Outlet Tubing SPE Cartridge Rack (24-Position) Collection and Drain Well Barbed Fitting Locator Plate (Rear) Figure 16 Flow to Waste Setup NOTE If your experiment does not require the full use of the 15- or 24-position rack, use plugs to fill the empty spaces. Refer to SPE Cartridge Plugs (Optional) on page 15. 22 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Setup for Flow to Collection 96-Position 1. Slide the locator plate to the front of the locator bed. 2. Move the drain well to the rear position of the locator plate. 3. Place the 96-position well plate on the front position of the locator plate. 4. Set the plate spacer on the 96-position well plate. 5. Set the appropriate SPE plate on the plate spacer. 15- or 24-Position 1. Slide the locator plate to the front of the locator bed. 2. Move the drain well to the rear position of the locator plate. 3. Place the 15- or 24 position tube rack with tubes on the front position of the locator plate. Locator Plate SPE Cartridge Rack (96-Position) Plate Spacer Collection and Drain Well Rear Figure 17 Flow to Collection Setup (96-Position) SPE Cartridge Rack (24-Position) Collection Tubes and Tube Rack 96-Position Well Plate Figure 18 Flow to Collection Setup (24-Position) (15-Position SPE Rack Not Shown) Front Operation 4. Set the appropriate 15- or 24-position SPE cartridge rack on the tube rack assembly. NOTE If your experiment does not require the full use of the 15- or 24-position rack, use plugs to fill the empty spaces. Refer to SPE Cartridge Plugs (Optional) on page 15. ASPEC Positive Pressure Manifold User's Guide 23

Operation Seat the Manifold 1. Push the manifold locking lever back to the fully unlocked position (Red Lock Symbol, unlocked). 2. Pull the manifold positioning lever forward to the fully raised position (toward the Up position). 3. Slide the locator plate back so that the SPE cartridges are directly below the manifold. NOTICE If you encounter interference with the safety shield, remove, and then replace the shield after positioning the locator plate. 4. Slowly push the manifold positioning lever back to lower the manifold (toward the Down position) until the manifold makes contact with the tops of the SPE cartridges. Rear Figure 19 Manifold Locking Lever Front Front 5. Pull the manifold locking lever forward to the fully locked position (Green Lock Symbol, locked) to create a seal between the manifold and the SPE cartridges. Rear Figure 20 Manifold Positioning Lever NOTICE Do not use the manifold positioning lever to tighten the seal. If the plate does not seat properly, unlock the manifold with the manifold locking lever, and then raise the manifold slightly with the manifold positioning lever. Repeat steps 1 through 5. Unseat the Manifold 1. Push the manifold locking lever back to the fully unlocked position (Red Lock Symbol, unlocked). 2. Pull the manifold positioning lever forward to the fully raised position (toward the Up position). 3. Slide the locator plate forward to the front of the locator bed. 24 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Control the Flow The ASPEC PPM features three different gas pressure controls (low flow, high flow, and dry) with fine tune adjustments available for low and high flow. The following provides a basic overview of control options. For step-bystep instructions, refer to page 28. Process Control Dial Low Flow Adjustment Knob Flow Adjustment Locks SPE Control Dial High Flow Adjustment Knob Operation Figure 21 Flow Controls Overview Flow Adjustment 1. Turn the adjustment knobs clockwise to open the valve and increase flow. 2. Turn the adjustment knobs counterclockwise to reduce flow and close the valve. The loss of tension in the adjustment knobs indicates that the valve is fully closed. High Flow Recommended for SPE cartridge wetting during conditioning and for washing. To turn on high flow: 1. Switch the process control dial to SPE. 2. Switch the SPE control dial to High Flow. 3. Turn the high flow adjustment knob clockwise until the flow reaches 4 to 5 drops per second. 4. To turn off high flow, switch the SPE control dial to Off. ASPEC Positive Pressure Manifold User's Guide 25

Operation Low Flow Recommended for conditioning (after initial SPE cartridge wetting with high flow), sample loading, and elution. To turn on low flow: 1. Switch the process control dial to SPE. 2. Switch the SPE control dial to Low Flow. 3. Turn the low flow adjustment knob clockwise until the flow reaches 1 to 2 drops per second. 4. To turn off low flow, switch the SPE control dial to Off. Dry Recommended for drying the SPE cartridges with maximum flow. To turn on the dry setting: 1. Ensure the SPE control dial is switched to Off. 2. Switch the process control dial to Dry. 3. To turn off the dry setting, switch the process control dial to SPE. NOTICE Turn off the manifold between process steps. Shut off the external gas supply when the manifold is not in use. Disconnect the manifold from the gas supply when storing the machine. 26 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

General Flow Guidelines The following table provides general process and flow guidelines. Table 1 SPE Process and Control Guidelines for SPE Steps SPE Steps NOTE Process Control Setting SPE Control Setting For all low and high flow recommendations, refer to the SPE Format Flow Guidelines table below. Condition SPE High Flow, and then switch to Low Flow Load SPE Low Flow, based on viscosity Wash SPE High Flow, based on viscosity Dry Dry Off Elute SPE Low Flow, based on viscosity Operation Table 2 SPE Format Flow Guidelines SPE Format High Flow (drops per second) 6 ml 3 to 5 1 Low Flow (drops per second) 3 ml 1 1 drop per 2 to 3 seconds 1 ml microplate 0.5 to 1 1 drop per 3 to 4 seconds ASPEC Positive Pressure Manifold User's Guide 27

Basic SPE Technique Operation 1. Ensure that the necessary conditions for operation are met. Refer to page 22. 2. Follow the instructions to Setup for Flow to Waste on page 22. Initial Condition Step 3. Pipette the appropriate volume of conditioning solvent into each available SPE cartridge. 4. Seat the manifold. Refer to Seat the Manifold on page 24. 5. Switch the SPE control dial to High Flow. 6. Turn the high flow adjustment knob clockwise until the desired flow rate is achieved. 7. When the solvent levels decrease to 2 mm above the fastest eluting cartridge of any one of the SPE cartridge/s, quickly switch the SPE control dial to Low Flow. Top Frit SPE Sorbent Bottom Frit Figure 22 SPE Cartridge Diagram 8. Turn the low flow adjustment knob clockwise until the flow slowly restarts. 9. When the solvent levels lower to the top frits of all of the SPE cartridges, quickly switch the SPE control dial to Off. Allow the solvent to return to atmospheric pressure. NOTE In some cases, positive pressure can remain in the SPE cartridges, even after the SPE control dial has been set to Off. Unseat the manifold to stop unwanted flow. Refer to page 24. 28 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Additional Condition Steps 10. Unseat the manifold. Refer to page 24. 11. Repeat steps 3 through 9 for the appropriate number of conditioning steps. NOTE Sample Load Steps If using an identical solvent for subsequent conditioning steps, use the flow adjustment locks to ensure the same pressure values are used. 12. Pipette the appropriate volume of sample into each available SPE cartridge. 13. Seat the manifold. Refer to page 24. 14. Switch the SPE control dial to Low Flow. 15. Turn the low flow adjustment knob clockwise until the desired flow rate is achieved. 16. When the sample stops dripping from the SPE cartridges, turn the SPE control dial to Off. 17. Unseat the manifold. Refer to page 24. Wash Steps 18. Pipette the appropriate volume of washing solvent into each available SPE cartridge. 19. Seat the manifold. Refer to page 24. 20. Switch the SPE control dial to High Flow. 21. Turn the high flow adjustment knob clockwise until the desired flow rate is achieved. 22. When the washing solvent stops dripping from the SPE cartridges, turn the SPE control dial to Off. 23. Unseat the manifold. Refer to page 24. 24. Repeat steps 18 through 23 for the appropriate number of washing steps. Operation ASPEC Positive Pressure Manifold User's Guide 29

Operation Dry Steps 25. Switch the process control dial to Dry. 26. When the solvent stops dripping from the SPE cartridges, wait an additional 10 seconds, and then switch the process control dial to SPE. 27. Unseat the manifold. Refer to page 24. Elution Steps 28. Follow the instructions to Setup for Flow to Collection on page 23. 29. Pipette the appropriate volume of eluent into each available SPE cartridge. 30. Switch the SPE control dial to Low Flow. 31. Turn the low flow adjustment knob clockwise until the desired flow rate is achieved. 32. When the eluate stops dripping from the SPE cartridges, turn the SPE control dial to Off. 33. Repeat steps 28 through 32 for the appropriate number of elution steps. 34. If needed, add additional dry steps. Final Steps 35. Eject the SPE cartridges. Refer to Ejection Plate on page 12. 36. Follow all necessary maintenance procedures after operation is complete. Refer to Maintenance on page 31. 30 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Maintenance Clean the ASPEC PPM The instrument should be cleaned occasionally, using a dry, clean cloth. If necessary, use a cloth dipped in soapy water. If liquid is accidentally spilled on the instrument, wipe it up immediately. Install or Replace the O-Ring 1. Remove the manifold from the manifold carrier. 2. Gently remove the O-ring from the rear of the manifold with your fingers. If necessary, free the O-ring with a flathead screwdriver. 3. Insert a new O-ring into the circular depression in the rear of the manifold. Replace the Manifold Gasket 1. Remove the manifold from the manifold carrier. 2. Set the manifold down with the gasket facing up. 3. Peel the gasket away, starting from the corner. Discard the gasket. 4. Clean off any excess adhesive from the manifold using methanol. 5. Locate the replacement gasket. 6. Peel away the adhesive backing on the new gasket, starting from the corner. Discard the backing material. 7. Align the new gasket with the four corners of the manifold before attaching the gasket with the adhesive side facing down. Maintenance Parts Description Part Number Gasket, 96-position for SPE manifold (qty. 10) 37417005 Gasket, 24-position for SPE manifold (qty. 10) 37417006 Gasket, 15-position for SPE manifold (qty. 10) 37417007 O-ring for manifold seal (qty. 5) 37417008 Maintenance ASPEC Positive Pressure Manifold User's Guide 31

Troubleshooting Table Symptoms Possible Causes SPE Steps Solutions No inlet pressure. Check that the gas pressure source is set to 15 psi. Troubleshooting Table Lack of flow Liquid flows unevenly O-ring damaged or missing. Replace the O-ring. Refer to page 31. All Damaged process control dial. Channeling inside the sorbent of the SPE cartridge/s. Clogged SPE cartridge/s. Condition Condition Load Replace the front panel. Contact your local Gilson representative. Refer to page 36. Specific Causes Drying of the cartridge/s. Insufficient condition volume. Excessive flow rate. Replace the SPE cartridge/s. Specific Solutions Repeat the condition step. Increase the condition volume. Reduce the flow rate. Reconsider the sample preparation workflow; e.g., sample filtration, centrifugation, etc. Troubleshooting Table Heterogeneous viscosity inside the SPE cartridge/s, caused by the use of different liquids in successive SPE steps. Condition Wash and Elute Reduce the residual level of liquid above the frit to 1 to 2 mm before conditioning with another type of liquid. Before using a new solvent, ensure that all effluent has been expelled from the SPE cartridges. Leak in the manifold gasket. All Replace the manifold gasket. Refer to page 31. Liquid continues to flow, even after the SPE control dial has been set to Off. The process control dial is set to Dry. Residual positive pressure remains in the SPE cartridge/s. All Switch the process control dial to SPE. Switch the SPE control dial to Low Flow before stopping. Unseat the manifold. Refer to page 24. 32 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD ASPEC Positive Pressure Manifold User's Guide 33

Symptoms Possible Causes SPE Steps Solutions Previous samples overflowed. Load Replace the manifold gasket. Refer to page 31. Troubleshooting Table Contamination Lower recoveries than usual for an optimized SPE protocol. Unclean collection tubes. Elution solvent splashed. SPE cartridge packing material dried. Not enough time for extraction to be completed. Residual trace of the washing solvent inside the packing material of the SPE cartridge/s prior to the elution step. Elution Condition Load Elution Wash Replace the collection vessels. Reduce the elution flow rate. When the liquid level on the fastest eluting SPE cartridge reaches 2 mm above the top frit (High Flow), switch to the SPE control dial to Low Flow, and then slowly turn the low flow adjustment knob clockwise until flow restarts and the liquid level equilibrates for all cartridges. Decrease the flow rate to better extract analytes from the sample matrices. Decrease the flow rate to better extract analytes from the solid phase. Switch the process control dial to Dry after the last washing step for several minutes. Troubleshooting Table Fewer interferents removed than usual for an optimized SPE protocol. Residual trace of the washing solvent inside the packing material of the SPE cartridge/s prior to the elution step. Not enough time to remove interferents. Wash Turn the process control dial to Dry after the last wash step. Thoroughly dry the SPE cartridges for several minutes. Decrease flow rate. A new batch of SPE cartridges. Elution Replace the SPE cartridges with a new batch. 34 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD ASPEC Positive Pressure Manifold User's Guide 35

Repair and Return Policies Repair and Return Policies Refer to the following information and then contact your local Gilson representative. Specific contact information can be found at www.gilson.com. Before Calling Us Your local Gilson representative will be able to serve you more efficiently if you have the following information: Serial number and model number of the instrument, located on the rear of the base. List of concise symptoms List of operating procedures and conditions you were using when the problem arose Warranty Repair Units covered under warranty will be repaired and returned to you at no charge. If you have any questions about applicability, contact your local Gilson representative. Non-Warranty Repair For out-of-warranty repairs, contact your local Gilson representative who will discuss service options with you and can assist in making arrangements to return the equipment, if necessary. 36 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Return Procedure Contact your local Gilson representative to obtain authorization before returning any Gilson equipment. To return a piece of equipment: Carefully pack the unit to prevent damage in transit. Check with your local Gilson representative regarding proper method of shipment. No responsibility is assumed by Gilson or your local Gilson representative for damage caused by improperly packaged instruments. Indicate the authorization on the carton and on the packing slip. Always insure for the replacement value of the unit. Include a description of symptoms, your name, address, phone number, and purchase order to cover repair costs, return and shipping charges, if your institution requires it. Unit End-of-Life When a unit reaches the end of its useful life, refer to www.gilson.com for directions and information on the end-of-life policy. This is in accordance with the European Union Directive 2002/96/EC on Waste Electrical and Electronic Equipment (WEEE). Repair and Return Policies ASPEC Positive Pressure Manifold User's Guide 37

Replacement Parts and Accessories Replacement Parts and Accessories Description Part Number 1 ml plugs for 24-position racks (qty. 24) 37417017 3 ml plugs for 24-position racks (qty. 24) 37417016 6 ml plugs for 15-position racks (qty. 15) 37417015 96-well collection plate, 1 ml (qty. 10) 543506004 96-well collection plate, 2 ml (qty. 10) 543506005 96-well plate adapter (qty. 1) 37114005 Collection and drain well (qty. 1) 37117000 Ejection plate for SPE cartridges (qty. 1) 37114006 External gas regulator, 15 psi (qty. 1) 37117100 Gasket, manifold, 96-positions (qty. 10) 37417005 Gasket, manifold, 24-positions (qty. 10) 37417006 Gasket, manifold, 15-positions (qty. 10) 37417007 Manifold, 96-positions (qty. 1) 37117296 Manifold, 24-positions (qty. 1) 37114000 Manifold, 15-positions (qty. 1) 37117215 O-rings, manifold seals (qty. 5) 37417008 SPE cartridge rack, 1 ml (qty. 1) 37114002 SPE cartridge rack, 3 ml (qty. 1) 37114003 SPE cartridge rack, 6 ml (qty. 1) 37114004 Safety shield (qty. 1) 37117200 Tubes, 12 x 75 mm, 5 ml, glass (qty. 250) 2954726 Tubes, 15 x 85 mm, 10 ml, glass (qty. 250) 2954729 38 USER S GUIDE ASPEC POSITIVE PRESSURE MANIFOLD

Configuration Kits Description Part Number 96-position 37417014 24-position, 1 ml 37417011 24-position, 3 ml 37417012 15-position, 6 ml 37417013 ASPEC Positive Pressure Unit Description Part Number ASPEC positive pressure unit 37012000 Configuration Kits ASPEC Positive Pressure Manifold User's Guide 39

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