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Table of Contents
Summary of Contents for SILICYCLE MiniBlock
- Page 1 SiliCycle MiniBlock® User Guide www.SiliCycle.com...
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Page 2: Table Of Contents
4.4.1.1. Securing SiliCycle MiniBlocks on the Shaking Station ....... . . - Page 3 Appendix C: SiliCycle MiniBlock Collection Rack Configurations ........
- Page 4 Figure 34: Examples of SiliCycle MiniBlock Collection Racks and Plates .......
- Page 5 Table 3: SPE Development Kits Available from SiliCycle ....... . .
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Page 6: Usage And Safety Precautions
1. Usage and Safety Precautions The SiliCycle MiniBlock products for parallel synthesis are intended for use by persons skilled in chemical handling and synthesis. Best results with the SiliCycle MiniBlock can be achieved by following the usage, maintenance and storage guidelines in this Operations Manual. -
Page 7: General
The SiliCycle MiniBlock’s patented valve mechanism enables simultaneous bottom drainage of all reaction vessels, aided by the use of vacuum and pressure. Reaction products are then transferred into collection vessels, or SPE tubes for purification. -
Page 8: The Silicycle Miniblock Reaction Tubes
2.1. The SiliCycle MiniBlock Reaction Tubes SiliCycle MiniBlock Reaction Tubes are designed as simple yet robust vessels for chemical synthesis. They consist of glass or polypropylene reaction tubes containing a 20 μm frit for solids filtration. Polyethylene Reaction Tube Cover Plate Septum Layer 20 µm Frit... -
Page 9: Figure 5: Types Of Pinch-Tube Inserts
(Figure 5). The Reaction Tubes are sealed at the bottom by compressing the Pinch-Tubes, which project through the SiliCycle MiniBlock (Figure 6). This closure is achieved for all Reaction Tubes simultaneously with a single turn of the T-handle valve key (Figure 7). -
Page 10: Silicycle Miniblock Configurations
2.2. SiliCycle MiniBlock Configurations The base SiliCycle MiniBlock comes as standard with 48 female luer fittings in the base. SiliCycle MiniBlock can be adapted to any of four basic configurations: Reaction Tubes Reaction Tube Reaction Tube Material Collection Format per SiliCycle MiniBlock... -
Page 11: Ambient Temperature Configurations
For temperature controlled reactions, heat transfer blocks are substituted for the alignment plates. The heat transfer blocks are color-coded, as are the alignment plates, except for the black heat transfer block, which is used with either a Blue or Red 48-Positions SiliCycle MiniBlock. The basic SiliCycle MiniBlock configurations with the heat transfer blocks are depicted in Figure 10. -
Page 12: Combining Red And Blue Silicycle Miniblocks Into 96-Well Format
2.3.2. Reaction Tube Materials 4 mL and 10 mL SiliCycle MiniBlock Reaction Tubes are available in either polypropylene or glass. The polypropylene tubes contain high quality polyethylene frits (average porosity: 20 μm). All glass Reaction Tubes (4, 10, 20 and 40 mL) have 20 μm average porosity frits. Glass reaction tubes also have a Teflon®... -
Page 13: Septa Materials
PFA Pinch-Tube Inserts. 2.3.4. Septa Materials The septa used to cover and seal the tops of SiliCycle MiniBlock reactors serve a number of different functions. They provide: • Sealing of the Reaction Tubes to minimize evaporation. -
Page 14: Silicycle Miniblock Temperature Control
Heat transfer fluid is recirculated through the anodized aluminum Heat Transfer Block, with heat transmitted efficiently. A different Heat Transfer Block is required for each of the four basic SiliCycle MiniBlock configurations (48, 24, 12 and 6-Positions) (Figure 10). Cover Plate... -
Page 15: Silicycle Miniblock Reactions Requiring An Inert Atmosphere
2.5. SiliCycle MiniBlock Reactions Requiring an Inert Atmosphere For air and / or moisture sensitive reactions, the SiliCycle MiniBlock can be fitted with an Inert Atmosphere Manifold (Figure 13). This manifold has a natural rubber septum inside, providing inert gas to individual reactor tubes. -
Page 16: Silicycle Miniblock Assembly And Reaction Setup
Pinch-Tube Inserts. See section 6.2.1 Replacement of Pinch-Tube Inserts for detailed instructions. 2. Use the T-handle Valve Key (5/32’’ hex key) to check that the valve mechanism slides freely (Figure 14). Be certain that the SiliCycle MiniBlock has been stored with the valve in the «open»... -
Page 17: Figure 15: Inspecting Pinch-Tubes
Figure 15: Inspecting Pinch-Tubes 3-5 mm Tall Tube Extender Collection Base Spacer Figure 16: Pinch-Tube Extension... -
Page 18: Silicycle Miniblock Assembly
3.2.2. Setup for Controlled Temperature Reaction 1. With no alignment plates on the SiliCycle MiniBlock, place a Heat Transfer Block of the corresponding color over the Alignment Pins. Be sure to orient the large alignment hole of the Heat Transfer Block with the large alignment pin on the SiliCycle MiniBlock. -
Page 19: Inserting Reaction Tubes
Figure 18: Heat Transfer Block Installed 3.2.3. Inserting Reaction Tubes 1. Insert the appropriate Reaction Tubes into the available positions on the SiliCycle MiniBlock (Figure 19). A full complement of Reaction Tubes is required; all positions must be occupied to assure uniform sealing. -
Page 20: Sealing For Reactions Not Requiring Inert Conditions
3.2.4. Sealing for Reactions Not Requiring Inert Conditions 1. Select the appropriate septum for your application (see section 2.3 SiliCycle MiniBlock System Materials). Multi-layer or laminated septa should be placed over Reaction Tubes with the Teflon® side down and the largest end notch fitted to the large alignment pin. -
Page 21: Figure 22: Septum Layer And Cover Plate
3. For multi-layer septa, place the black settling mat on top of the reaction tubes. 4. Cover with the Top Plate and close both side clamps simultaneously (Figure 22). This will firmly seat the reaction tubes. Cover Plate Septum Layer Spring Clamp Large Alignment Pin Figure 22: Septum Layer and Cover Plate... -
Page 22: Sealing For Reactions Requiring Inert Conditions
This will seat the luer fittings at the bottom of the Reaction Tubes and seal the top of the Reaction Tubes to prevent evaporation. 4. With the SiliCycle MiniBlock valve open, purge the Reaction Tubes with inert gas for a sufficient period to completely displace all air. -
Page 23: Closing The Silicycle Miniblock Valve
3.2.6. Closing the SiliCycle MiniBlock Valve SiliCycle MiniBlock Reaction Tubes should be closed just prior to the onset of reagent addition. Close the valve mechanism by inserting the Valve Key into the actuator screw (Figure 24) and turning clockwise until the screw is firmly seated. Do not over tighten. A good guide for the correct amount of torque is to turn the valve until the left side of the reactor lifts from the work surface. -
Page 24: Reaction Setup, Mixing And Incubation
Kan scanning and sorting into SiliCycle MiniBlocks. 4.1.4. Resin Swelling Resin conditioning and swelling prior to synthesis can be readily accomplished in a SiliCycle MiniBlock. See section 5 Washing, Purification and Product Collection for information regarding washing operations on the SiliCycle MiniBlock. -
Page 25: Adding Solvents And Reagents
Air sensitive materials may also be added to the SiliCycle MiniBlock in a glove bag or other inert atmosphere handling enclosure. Close down the Inert Atmosphere Manifold on the SiliCycle MiniBlock while still in the glove bag and use suitable techniques to assure a continual inert environment for the reactions. -
Page 26: Reaction Mixing And Incubation
4.4.1.1. Securing SiliCycle MiniBlocks on the Shaking Station Position SiliCycle MiniBlocks by locating them on shaker alignment pins (Figure 27). To secure the SiliCycle MiniBlocks, turn the hex screws in the shaker top clamps clockwise (Figure 28) using the supplied T-handle Valve Key. Tighten the clamps down on to the notches on each side of the reactor. -
Page 27: Pre-Operational Shaking Station Check
4.4.1.3. Pre-Operational Shaking Station Check Apply a vacuum to the fitting at the rear of the shaker. To obtain a good vacuum seal, all SiliCycle MiniBlock positions need to be covered with a reactor or a counterweight (double shaker). If you do not obtain adequate vacuum suction, check the following: •... -
Page 28: Setting Agitation Speed
4.5. Incubation Each SiliCycle Shaking Station has a site for a Recirculator Manifold. These heat transfer fluid distribution manifolds are connected to a temperature controlled recirculator unit. SiliCycle MiniBlock Heat Transfer Blocks receive heat transfer fluid from the Recirculator Manifold. -
Page 29: Connecting To The Recirculator
It is normal for one or two drops of recirculating fluid to drip when engaging or disengaging. Do not continue if there is a leak at any time. WARNING: For temperatures exceeding 80°C, high temperature components MUST be used. Contact SiliCycle for more information. -
Page 30: Washing, Purification And Product Collection
Connect a vacuum line (with an in-line trap for solvents) to the connector on the back of the shaker top. Open the SiliCycle MiniBlock slide valve before pulling a vacuum. The valve opens by turning the actuator screw counterclockwise two full turns. -
Page 31: Air Push Assist Device
The Positive Pressure Manifold is clamped on top of the reaction tubes and replaces the standard Cover Plate. Once connected to an air or nitrogen line, the Positive Pressure Manifold applies pressure to all 48 reaction vessels at the same time. The manifold may be left clamped on the SiliCycle MiniBlock throughout the reaction procedure, e.g. -
Page 32: Inert Atmosphere Manifold
5.2.1. Solid-Phase Extraction (SPE) Following synthesis, the reaction products can be purified by a simple transfer into a second SiliCycle MiniBlock, or a filter plate containing SPE packing by stacking two SiliCycle MiniBlocks (Figure 33). An Inert Atmosphere Manifold, or Positive Pressure Manifold is required to push the reaction products from the top SiliCycle MiniBlock through the Transfer Adapter (containing an Adapter Plate) into the second SiliCycle MiniBlock containing the SPE packed tubes. -
Page 33: Scavenger Resins
Clean-up following synthesis can be expedited through use of scavenger resins. Simply dispense the appropriate amount of resin into each reaction tube. A new Resin Dispenser, capable of accurately dispensing various resin quantities is now available (13822001). The SiliCycle MiniBlock Resin dispenser is designed to evenly dispense resin to 48 Reaction Tube positions simultaneously. -
Page 34: Collection Rack Selection
To collect / cleave products, place the appropriate collection rack / plate inside the Vacuum Collection Base (Figure 35). Place the SiliCycle MiniBlock on top of the Vacuum Collection Base, ensuring proper alignment of locating pins. Open the valve and turn on the vacuum to collect products into the rack / plate (Figure 36). - Page 35 • Collection racks are available for a variety of test tubes and vials for each SiliCycle MiniBlock position configuration. • Collection racks are available in Aluminum or UHMW (Ultra-high MW Polyethylene). In general, the aluminum racks are heavier than UHMW racks, but aluminum has superior heat transfer properties.
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Page 36: Table 4: Collection Plates, Racks And Vessels
Glass 15 mL Test Tube, 16 mm D x 100 mm H 13521108 Glass 15 mL Vial, 21 mm D x 70 mm H 13521114 Glass 55 mL Scintillation Vial, 28 mm D x 135 mm H Table 4: Collection Plates, Racks and Vessels www.SiliCycle.com | info@SiliCycle.com SiliCycle MiniBlock® User Guide... -
Page 37: Collection Vessel Positioning
The SiliCycle MiniBlock collection system also includes Tube Extenders and Spacers (Figure 37). The purpose of these components is to shim the top of the collection vessels to a height just below the bottom of the SiliCycle MiniBlock (Figure 38). A Tube Height Gauge is now available to aid determine the correct height for collection tubes. -
Page 38: Figure 38: Positioning Silicycle Miniblock Components For Collecting Into 48 Test Tubes Rack
For Collecting Into 48 Test Tubes Rack TECH TIP: When the collection tube heights are properly set, the Pinch-Tubes from each SiliCycle MiniBlock Reaction Tube actually project into the collection tubes. This tube proximity is key to preventing cross- contamination during the collection process. (Figure 39) The available options for Extenders and Spacers are listed in Table 8. -
Page 39: Maintenance
6. Maintenance The results you can achieve with the SiliCycle MiniBlock system for parallel synthesis are dependent on the condition of your equipment. As with any equipment in a multi-user laboratory environment, attention to cleanliness and proper equipment function must be built into routine laboratory processes to assure maximum efficiency. -
Page 40: Silicycle Miniblock Cleaning
8. Tilt the SiliCycle MiniBlock over a waste vessel in a fume hood. Using a suitable solvent wash bottle, rinse all female luer fittings and use vacuum (shaking / washing station or collection base) to pull solvent through the block. Inspect and manually wipe off particulates. Repeat as necessary. -
Page 41: Figure 41: Remove Valve Insert Lock-Plate
Valve Insert Lock-Plate Figure 41: Remove Valve Insert Lock-Plate 4. The Pinch-Tube Inserts can now be pulled out; pull them straight out and discard. If a Pinch-Tube Insert does not come out easily, extract it with the needle nose pliers (Figure 42). Figure 42: Remove Pinch Tube Inserts 5. -
Page 42: Replacement Of Compression Cords
Pinch-Tube over it and ease the Pinch-Tube Insert into the base from the top. 7. When all Pinch-Tube Inserts have been replaced, turn the block over and inspect the extension of the Pinch-Tubes from the SiliCycle MiniBlock base. -
Page 43: Troubleshooting
Excessive evaporation can be caused by tube height unevenness. Worn Pinch-Tube Inserts (female luers) can cause this, as the Reaction Tubes sink too far down into the luer fitting. Leaving SiliCycle MiniBlocks clamped for extended periods can also cause Reaction Tubes to sink too far into the luer fittings. - Page 44 Corrective Action: marked with a large green dot. The green dot indicates that they have passed SiliCycle quality control tests. Leakage at the luer fitting has also resulted from improper formation of the male luer fitting on glass reaction tubes. Glass reaction tubes should have a blue Teflon® shrink-wrap on the luer fitting to facilitate a tight fit and luer joint sealing.
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Page 45: Preventive Maintenance
SiliCycle MiniBlock’s maintenance requirement for a given lab can be influenced by usage pattern, chemistry used, temperatures, handling and cleaning techniques, etc. By tracking SiliCycle MiniBlock usage in a log, a pattern will emerge which will help establish a preventive maintenance schedule and maximize utilization of the SiliCycle MiniBlock technology. -
Page 46: Figure 45: Exploded View Of Silicycle Miniblock Reactor
Reaction Tube (Red) Pinch Tube Insert (Red) Figure 45: Exploded View of SiliCycle MiniBlock Reactor www.SiliCycle.com | info@SiliCycle.com SiliCycle MiniBlock® User Guide... -
Page 47: Table 5: Silicycle Miniblock Spare Parts
13260336 Bottom Plate 13260340 End Cap 13260344 Latch Pivot Block 13260442 #10-32, 3/4” Long SHCS, (Lubricated) 13260346 Vacuum Plate, Red 13223100 #10-32, 3/4” Long SHCS, SS 13221024 #4-40, 3/4” Long Flat Head Screw, SS Table 5: SiliCycle MiniBlock Spare Parts... -
Page 48: Appendix A: Heat Shrinking Teflon® Sleeves Onto Glass Reaction Tubes
If you encounter problems in carrying out the instructions, contact Customer Service (+1 877 745-4292, North America Only, or +1 418 874-0054, for the rest of the world, or send us an e-mail at MiniBlock@SiliCycle.com). 1. Place tubes, luer end up in the appropriate metal rack (a plastic racks will melt). -
Page 49: Quality Checks
A.3. Quality Checks A.3.1. Incomplete Heat-Shrinking If the sleeve is not tightly shrunk around the luer tip, re-heating may be required to complete the process. To do this, place the tube back in the oven for five (5) more minutes at 350°C. If the problem is not corrected by the second attempt, remove the sleeve and start from the beginning. A.3.2. -
Page 50: Appendix B: Resin Dispenser: Operating Instructions
The dispensing plates have wells with exact volumes, allowing various quantities of resin or other freeflowing powders to be dispensed. The dispensing plates adapt to Red or Blue SiliCycle MiniBlocks, by inserting the corresponding side of the plate, based on which color block is being used. -
Page 51: Dispensing
B.3. Dispensing B.3.1. Resin Dispenser Setup (Procedure written for the 48-Positions Version) 1. Line up the large SiliCycle MiniBlock post with the large hole and place the resin dispenser body onto a SiliCycle MiniBlock. Item Description Resin Dispenser Base, with Quick Release Pin... -
Page 52: Dispensing Procedure
Make several passes if necessary, to ensure the powder is evenly distributed to the openings. 4. Spread the excess powder back into the recessed surface next to the slot in the resin dispensing plate. Figure 50: Resin Dispensing Spreader www.SiliCycle.com | info@SiliCycle.com SiliCycle MiniBlock® User Guide... -
Page 53: Dispensing To Microtiter / Deep Well Plates
1. Choose either a Red or Blue SiliCycle MiniBlock without reaction vessels. Remove both alignment plates and the Top Plate. 2. Place the microtiter plate adapter onto the SiliCycle MiniBlock by lining up the large hole with the large post. Take care to install the microtiter plate adapter with the correct side up, as indicated by the color-coded marking on the adapter. -
Page 54: Resin Cleaning
1. Tare weigh twelve (12) SiliCycle MiniBlock reaction vessels. 2. Install the pre-weighed reaction vessels into a SiliCycle MiniBlock. For a Red block, the positions will be F-2, F-4, F-6… F-12 and H-2, H-4, H-6… H12. For a Blue block, the positions will be F-1, F-3, F-5… F-11 and H-1, H-3, H-5… H-11. -
Page 55: Appendix C: Silicycle Miniblock Collection Rack Configurations
Appendix C: SiliCycle MiniBlock Collection Rack Configurations The following tables and diagrams depict the appropriate assembly of components for collection into the Vacuum Collection Base. The Vacuum Collection Base Set (see Figure 53) contains one Black and one White Spacer, plus the new Tube Height Gauge. -
Page 56: Assembly Diagrams
Figure 55 : 12 x 75 mm Test Tubes (6 mL) Tall Tube Extender Collection Rack White Spacer Vacuum Base Figure 56 : Deep Well Plate Figure 57 : Tall Minitube Rack (2.5 mL) (Various Volumes) www.SiliCycle.com | info@SiliCycle.com SiliCycle MiniBlock® User Guide... -
Page 57: Figure 58 : 16 X 100 Mm Test Tubes (15 Ml)
Tall Tube Extender Collection Rack Black Spacer Vacuum Base Figure 59 : 15 x 45 mm Vials (3.7 mL) Figure 58 : 16 x 100 mm Test Tubes (15 mL) Tall Tube Extender Collection Rack White Spacer Vacuum Base Figure 61 : 21 x 70 mm Vials (15 mL) Figure 60: 17 x 61 mm Vials (7.5 mL) Tall Tube Extender Collection Rack... -
Page 58: Appendix D: Determining Correct Collection Tube Height
1. All Pinch-Tubes should project 3 to 5 mm from the bottom of the SiliCycle MiniBlock base. 2. The collection tube tops need to be just below the SiliCycle MiniBlock base (within 1 mm). Achieving this height is dependent on using the right combination of collection racks, tubes, spacers and tall tube extenders. -
Page 59: Appendix E: Chemistry Applications
Solution-Phase Parallel Synthesis of Hexahydro-1H-Isoindolone Libraries SiliCycle MiniBlock XT is extremely useful for complex, multi-step synthesis protocols where a variety of volumes and reaction conditions are needed. Several steps in the synthesis described below were run at reflux and under inert conditions. Multiple steps required different scales and a variety of reaction arrays to be used. - Page 60 At SiliCycle, we are at the forefront of the chromatography industry, owing to the extraordinary purity of our silica gels and polymeric sorbents, combined with our capacity to rapidly adapt our products to meet the specific requirements of scientists worldwide.
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