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SiliCycle MiniBlock® User Guide

46

www.SiliCycle.com | [email protected]

Figure 45: Exploded View of SiliCycle MiniBlock Reactor

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(Red)

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Reaction Tube

Pinch Tube Insert

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Содержание MiniBlock

Страница 1: ...www SiliCycle com SiliCycle MiniBlock User Guide ...

Страница 2: ...Reaction Setup 16 3 1 Pre AssemblyChecks 16 3 2 SiliCycleMiniBlockAssembly 18 3 2 1 Setup for Ambient Temperature Reaction 18 3 2 2 Setup for Controlled Temperature Reaction 18 3 2 3 Inserting Reaction Tubes 19 3 2 4 Sealing for Reactions Not Requiring Inert Conditions 20 3 2 5 Sealing for Reactions Requiring Inert Conditions 22 3 2 6 Closing the SiliCycle MiniBlock Valve 23 4 Reaction Setup Mixin...

Страница 3: ...40 6 2 2 Replacement of Compression Cords 42 7 Troubleshooting 43 7 1 JammedSlideValve 43 7 2 Leakage SolventLoss 43 7 3 PreventiveMaintenance 45 Appendix A Heat Shrinking Teflon Sleeves Onto Glass Reaction Tubes 48 A 1 Apparatus 48 A 2 Procedure 48 A 3 QualityChecks 49 A 3 1 Incomplete Heat Shrinking 49 A 3 2 Defective Heat Shrinking 49 Appendix B Resin Dispenser Operating Instructions 50 B 1 Ove...

Страница 4: ...te 21 Figure 23 Inert Purge Manifold 22 Figure 24 SiliCycle MiniBlock With Valve Key 23 Figure 25 Dispensing Plate 24 Figure 26 Shaking Stations 26 Figure 27 Aligning SiliCycle MiniBlocks on the Shaker Top With Optional Recirculator Manifold 27 Figure 28 Securing SiliCycle MiniBlocks on the Shaker Top 27 Figure 29 Attaching the Recirculator Manifold to the Shaker Top 28 Figure 30 Slide Valve Opera...

Страница 5: ... 5 mL 56 Figure 58 16 x 100 mm Test Tubes 15 mL 57 Figure 59 15 x 45 mm Vials 3 7 mL 57 Figure 60 17 x 61 mm Vials 7 5 mL 57 Figure 61 21 x 70 mm Vials 15 mL 57 Figure 62 28 x 95 mm Vials 40 mL 57 Figure 63 Tube Heights are Correct GO 58 Figure 64 Tube Heights are too Low NO GO 58 Figure 65 Tube Heights are too High NO GO 58 Tables Table 1 MinBlock Physical Description 7 Table 2 SiliCycle MiniBloc...

Страница 6: ...nance program Storage SiliCycle MiniBlocks should be stored with the slide drainage valve in the open position and the two side clamps left undone Temperature Reaction temperatures are limited to 80 C unless high temperature components are obtained from SiliCycle Reaction temperatures must be achieved using the apparatus described in this manual Pressure SiliCycle MiniBlocks are not designed to wi...

Страница 7: ...ultaneous 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 Ancillary components are used to achieve reaction agitation and temperature control for the SiliCycle MiniBlock system Height Width Depth Weight 5 13 cm 7 18 cm 5 13 cm 6 4 lbs 2 9 kg Table 1 MinBlock Physical Descrip...

Страница 8: ...igure 3 SiliCycle MiniBlock Components Polyethylene Reaction Tube Cover Plate Septum Layer Upper Alignment Plate Lower Alignment Plate Blue Teflon Heat Shrink Sleeve Large Alignment Pin Small Alignment Pin Reaction Tube 20 µm Frit Pinch Tube Female Luer Fitting Male Luer Fitting Glass reaction tubes also have a Teflon heat shrink sleeve at the luer tip to improve sealing When using toluene or othe...

Страница 9: ... 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 PFA Teflon Grey Fittings Figure 6 Valve Mechanism in Closed Position Figure 7 SiliCycle MiniBlock with Valve Key Figure 5 Types of Pinch Tube Inserts ...

Страница 10: ...ns 24 Green Block 10 Glass 24 positions 12 Silver Block 20 Glass 12 positions 6 Gold Block 40 Glass 6 positions Table 2 SiliCycle MiniBlock Configurations SiliCycle MiniBlock configurations together with the reaction tubes and color coding are depicted in Figure 8 Glass reaction tubes are provided with a blue Teflon heat shrink sleeve at the luer tip This is to improve sealing against the female l...

Страница 11: ...r 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 TECH TIP The two 2 different 48 Positions SiliCycle MiniBlocks Red and Blue are actually complementary configurations A Blue block c...

Страница 12: ...y resistant to chemicals and physical wear 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 heat shrink sleeve at the ...

Страница 13: ...cept those exceeding 80 C Silicone Multi Layer Septa 13742080 for reactions requiring high temperatures up to 160 C TECH TIP SiliCycle MiniBlocks are not designed for pressurized reactions Do not perform synthesis at or above solvent boiling points Pressure buildup resultant from synthesis can be avoided using an Inert Atmosphere Manifold See Section 3 2 5 Sealing For Reactions Requiring Inert Con...

Страница 14: ... Figure 12 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 Heat Transfer Block Locking Arm Large Alignment Pin Small Alignment Pin Quick Disconnect Fitting Septum Layer Cover Plate Figure...

Страница 15: ...tor tubes The Inert Gas Manifold septum can also be pierced at each reactor position with a syringe without compromising the inert conditions in the reactors Figure 13 Inert Purge Manifold MiniBlock Format Inert Manifold PN Internal Septum PN Sealing Gaskets Bottom Gasket Rubber PN Multi Layer PN 6 positions 13200957 13742152 13200992 13201040 12 positions 13200951 13742169 13200993 13201041 24 po...

Страница 16: ... 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 position If the valve was closed see section 6 Maintenance before proceeding 3 Inspect the Pinch Tubes the part of the Pinch Tube Inserts which projects through the base of the SiliCycle MiniBlock on the bottom of the SiliCycle MiniBlock Fig...

Страница 17: ...17 Figure 15 Inspecting Pinch Tubes Figure 16 Pinch Tube Extension Tall Tube Extender Spacer 3 5 mm Collection Base ...

Страница 18: ...liCycle MiniBlock Red and Blue SiliCycle MiniBlocks require a Black 48 Positions Heat Transfer Block The 24 12 and 6 Positions SiliCycle MiniBlocks have color coded Heat Transfer Blocks Green for 24 Positions Silver for 12 Positions Gold for 6 Positions 2 Secure the Heat Transfer Blocks on either side of the SiliCycle MiniBlock using front and back locking arms and thumbscrews Figure 18 TECH TIP T...

Страница 19: ...ittings of the Pinch Tube Inserts Figure 20 The luer fittings are compressed together by installation of the septum and cover plate or inert atmosphere manifold Upper Alignment Plate Heat Transfer Block Reaction Tube Reaction Tube Small Alignment Pin Heat Transfer Block Lower Alignment Plate Thumb Screw Front Locking Arm Large Alignment Pin Large Alignment Pin Figure 18 Heat Transfer Block Install...

Страница 20: ...laminated septa should be placed over Reaction Tubes with the Teflon side down and the largest end notch fitted to the large alignment pin 2 Place the appropriately colored cover plate over the Reaction Tubes being careful to correctly orient the plate on the large alignment pin Figure 21 Reaction Tube Female Luer Fitting Valve Insert Spring Clamp Lower Alignment Plate Upper Alignment Plate Figure...

Страница 21: ...firmly seat the reaction tubes Cover Plate Septum Layer Large Alignment Pin Spring Clamp Figure 22 Septum Layer and Cover Plate 5 Leave clamped for at least 30 seconds before removing the settling mat 6 Place the multi layer septum making sure the septum is oriented correctly and that the clear Teflon layer is at the bottom Figure 23 7 Close both spring clamps and begin use ...

Страница 22: ...k simultaneously to lock down the Inert Atmosphere Manifold Figure 23 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 Inert Purge Manifold 48 positions Septum Layer Large Alignment...

Страница 23: ...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 The SiliCycle MiniBlock is now ready for use Figure 24 SiliCycle MiniBlock With Valve Key CAUTION The indicator button on the front of the SiliCycle MiniBlock is in the Out position whe...

Страница 24: ...nned in manually and placed into Reaction Tubes For unattended operation the IRORI AutoSort 10KX can be used to automate 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 ...

Страница 25: ...ontinual inert environment for the reactions 4 3 Adding Solvents and Reagents Solvents and reagents can be added with or without the septum layer Addition can be via syringe pipette or a liquid handler Syringe additions can also be accomplished through the septum with the Inert Atmosphere Manifold TECH TIP Solvent and Reagent additions to a SiliCycle MiniBlock can be automated using Neptune or USP...

Страница 26: ...MiniBlocks Vacuum assisted drainage to waste for washing Balance for reduced noise and vibration The SiliCycle Shaking Stations holds up 1 or 2 SiliCycle MiniBlocks Figure 26 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 cl...

Страница 27: ...the following Make sure all the sealing surfaces are clean and free of dust and particles Make sure all connectors fittings around the shaker top are tight and leak free Make sure valves on all the SiliCycle MiniBlocks are closed properly If required isolate an individual Reactor by plugging the other positions with the plugs provided Figure 27 Aligning SiliCycle MiniBlocks on the Shaker Top With ...

Страница 28: ... the Shaker Top TECH TIP The heat transfer fluid recirculator must perform to specifications e g heat capacity pressure consistent with SiliCycle MiniBlock system design The recirculator unit should be purchased from or approved by SiliCycle WARNING Use only open bath style recirculators with the SiliCycle MiniBlock system Consult SiliCycle with any questions on recirculator selection Do not place...

Страница 29: ... the manifold tube While pushing in the spring loaded button on the female connector gently push the fitting together and release the button Failure to depress the button while connecting the fitting can result in damage to the fitting and leakage of heat transfer fluid 4 5 3 Testing the Recirculation System Follow the directions of the manufacturer Turn recirculator on and make sure there are no ...

Страница 30: ...tuator screw counterclockwise two full turns It is not necessary to turn the screw further than two full turns to apply a vacuum The waste will be drawn into the solvent collection trap by the vacuum Solvents drain more quickly if you remove the Top Plate and septum during washing The immediate cleanup of the solvent waste station is recommended after SiliCycle MiniBlocks have been removed WARNING...

Страница 31: ...you may use the Positive Pressure Manifold Figure 32 The Positive Pressure Manifold is used in other applications such as block to block transfers and SPE purification 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...

Страница 32: ...ing station 5 2 Purification and Clean Up 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 ...

Страница 33: ...g 4 5 mL 6 Each Phase HLB DVB SCX WCX SAX WAX KSPMB K2003 100P SiliaPrepX MB Polymeric Development Kit 500 mg 10 0 mL 3 Each Phase HLB DVB SCX WCX SAX WAX Table 3 SPE Development Kits Available from SiliCycle 5 2 2 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 Dispen...

Страница 34: ...s which require the use of corrosive reagents such as TFA Promptly clean all surfaces in contact with such agents Vacuum Collection Base Figure 36 Vacuum Collection Base Shown With a 24 Positions Rack 5 3 1 Collection Rack Selection The SiliCycle MiniBlock is designed to be a flexible platform for product collection Collection racks are available to accommodate most common container types and size...

Страница 35: ...uminum racks are heavier than UHMW racks but aluminum has superior heat transfer properties The rack material should be chosen to fit the requirements of the evaporator to be used Consult the manufacturer of your evaporator for guidelines when selecting collection racks TECH TIP All SiliCycle MiniBlocks have either a Blue or Red bottom plate The color of this plate dictates the color of the approp...

Страница 36: ... H 24 13260457 13260487 Red Rack for 15 mL Test Tube 16 mm D x 100 mm H 24 13260432 13260476 Blue Rack for 15 mL or 23 mL Vial 21 mm D x 70 mm H or 21 mm D x 112 mm H 12 13260431 13260477 Red Rack for 15 mL or 23 mL Vial 21 mm D x 70 mm H or 21 mm D x 112 mm H 12 13260460 13260478 Blue Rack for 38 mL or 45 mL Test Tube 24 mm D x 112 mm H or 24 mm D x 150 mm H 12 13260461 13260479 Red Rack for 38 m...

Страница 37: ...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 Figure 37 Proper Height Alignment for Collection Tubes Positive Pressure Manifold Septum Layer Test Tube Rack Vacuum Base Reaction Tube Tall Tube Extender Test Tube Black Spacer ...

Страница 38: ... Extenders are indexed to fit into the vacuum collection base in the proper orientation Test Tube Extender Vacuum Base 9 12 mm 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 Figure 39 ...

Страница 39: ...Shaking Station or empty vacuum base 3 Add suitable cleaning solvent to all Reaction Tubes 4 Open the Reactor Valve 5 Using vacuum and air pressure as needed drain solvent to waste 6 Repeat steps 3 to 5 until residual cleavage agents reaction by products etc are sufficiently diluted 7 Remove the tubes If using polypropylene tubes Reaction Tube removal can be aided by use of the Tube Removal Tool F...

Страница 40: ...2 Do not use acetone 3 Immerse the SiliCycle MiniBlock in enough solvent to cover all the Pinch Tube Inserts 4 Sonicate two to five 5 minutes 5 Wipe off excess solvent 6 Dry the SiliCycle MiniBlock with a stream of nitrogen or air and inspect 7 Test the sliding valve mechanism 8 Repeat steps 3 to 7 as necessary 9 Leave the Reactor slide valve mechanism Open for storage 10 Do not reuse the solvent ...

Страница 41: ... out and discard If a Pinch Tube Insert does not come out easily extract it with the needle nose pliers Figure 42 Valve Insert Lock Plate Figure 42 Remove Pinch Tube Inserts 5 If Compression Cords for the Pinch Tube Inserts are to be replaced it should be done while all Pinch Tube Inserts are out of the block ...

Страница 42: ... the keys securing the four 4 retaining screws 6 2 2 Replacement of Compression Cords 1 Remove all Pinch Tube Inserts 2 Remove the eight 8 sets of hex screws at each end of the SiliCycle MiniBlock base Figure 43 using the T handle Valve Key Figure 43 Compression Cords Replacement 3 The eight 8 Compression Cords can be replaced by sequentially pushing each used cord out of one end using a new Compr...

Страница 43: ...tion 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 Corrective Action Worn Valve Inserts should be replaced Solvent loss at the top of the Reaction Tubes can also be ...

Страница 44: ...ple positions simultaneously more force is required to close a flattened tube amid newer tubes which are dimensionally sound Corrective Action Replace any Pinch Tube Inserts which leak in spite of normal closure see section 3 2 6 Closing The SiliCycle MiniBlock Valve Periodically replace all Pinch Tube Inserts to improve closure force evenness The Compression Cords which close the Pinch Tube may l...

Страница 45: ...od is as follows 1 Start with a clean dry SiliCycle MiniBlock containing no Reaction Tubes The Reactor Valve should be Open 2 Inspect the bottom side of the reactor to see that the Pinch Tubes all extend 3 to 5 mm from the bottom Replace any Pinch Tube Inserts that do not extend the proper distance 3 Close the Reactor Valve 4 Fill each open luer with isopropanol from a squirt bottle Tip the reacto...

Страница 46: ...iliCycle com info SiliCycle com Figure 45 Exploded View of SiliCycle MiniBlock Reactor 1 4 5 6 11 20 21 22 32 27 35 Red 7 18 29 2 12 13 14 15 16 6 23 24 27 34 25 26 30 36 33 3 Red Reaction Tube Pinch Tube Insert 8 9 10 17 37 27 27 28 19 31 ...

Страница 47: ...18 13260369 1 Indicator 19 13260342 2 Clamp Bracket 20 13223021 2 4 40 3 4 Long SHCS SS 21 13260345 1 Side Latch Front 22 13226036 2 Shoulder Screw 1 8 DIA x 1 8 Long SST 1 8 4 40 Thread 23 13221098 4 10 32 3 4 Long Flat Head Screw SS 24 13260338 1 Top Plate 25 13217003 4 Split Lock Washer 6 SS 26 13223098 9 10 32 1 2 Long SHCS SS 27 13260441 16 10 32 1 2 Long SHCS 28 13260395 8 PTFE Coated Compre...

Страница 48: ...e com 1 Place tubes luer end up in the appropriate metal rack a plastic racks will melt 2 Cut approximately 8 mm sections of the heat shrink tubing ensuring a square cut When placed on the luer the Teflon sleeve should leave 1 1 5 mm of the ground glass tip uncovered The bottom end of the sleeve should rest on the shoulder of the glass tube The glass tip has some variations in length of the luers ...

Страница 49: ...and start from the beginning A 3 2 Defective Heat Shrinking In cases where the sleeve is split melted or misplaced remove the Teflon and apply new material In order to spot more minor imperfections grasp the luer between two fingers and rotate the reaction tube If the Teflon sleeve is applied correctly it will be smooth to the touch If imperfections are felt small areas where the Teflon did not sh...

Страница 50: ...ich color block is being used A color coded tag is located on each plate indicating the correct plate side to be used Figure 47 Resin Dispensing Plate Beveled End Slot Closed Position Large Alignment Pin Quick Release Pin Spring Loaded Rectangle Dispensing Plate Color Coding Must Face Up Hard Stop The dispensing plates are inserted under the spring loaded rectangle base then locked into place by a...

Страница 51: ...Table 7 High Volume Kit Sold Separately 2 Select the dispensing plate with the desired dispensing volume and insert the beveled end of the plate between the resin dispenser base and the spring loaded rectangle 3 Lock the resin dispensing plate in place by inserting the quick release pin into the tab If the tab and the slot do not line up turn over the dispensing plate and insert the correct side s...

Страница 52: ...l the wells 3 Using the resin dispensing spreader distribute the powder across the openings in the resin dispensing plate by evenly spreading the powder across the dispensing plate 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 Dispen...

Страница 53: ...e powders to microtiter plates A Red or Blue SiliCycle MiniBlock is needed to ensure everything lines up correctly Figure 51 To dispense to microtiter 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 c...

Страница 54: ...on Calibration is recommended to correlate the exact mass dispensed to the fixed volume of the dispensing plates The following is a simple procedure using the calibration plate and the 4 5 mL polypropylene SiliCycle MiniBlock reaction vessels 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 positio...

Страница 55: ... Vials 3 7 mL 0 0 13260443 13260473 24 Red 15 x 45 mm Vials 3 7 mL 0 0 13260430 13260474 24 Blue 17 x 61 mm Vials 7 5 mL 1 0 13260429 13260475 24 Red 17 x 61 mm Vials 7 5 mL 1 0 13260456 13260486 24 Blue 16 x 100 mm Test Tubes 15 mL 2 1 13260457 13260487 24 Red 16 x 100 mm Test Tubes 15 mL 2 1 13260432 13260476 12 Blue 21 x 70 mm Vials 15 mL 1 0 13260431 13260477 12 Red 21 x 70 mm Vials 15 mL 1 0 ...

Страница 56: ... Diagrams Tall Tube Extender Tall Tube Extender Collection Rack Collection Rack Black Spacer White Spacer Vacuum Base Vacuum Base Figure 54 12 x 100 mm Test Tubes 8 mL Figure 56 Deep Well Plate Various Volumes Figure 55 12 x 75 mm Test Tubes 6 mL Figure 57 Tall Minitube Rack 2 5 mL ...

Страница 57: ...ollection Rack Collection Rack Black Spacer Black Spacer White Spacer Vacuum Base Vacuum Base Vacuum Base Figure 58 16 x 100 mm Test Tubes 15 mL Figure 60 17 x 61 mm Vials 7 5 mL Figure 62 28 x 95 mm Vials 40 mL Figure 59 15 x 45 mm Vials 3 7 mL Figure 61 21 x 70 mm Vials 15 mL ...

Страница 58: ... rack collection tubes and a tall tube or tall tube double extender as needed 2 Place the Collection Tube Height Gauge on top of the vacuum base or extender ensuring the arrows point toward the collection tubes 3 Slide the gauge toward the tube tops Tube heights too high NO GO Tube Heights too Low NO GO TECH TIP Collection Tube tops are shimmed to the proper height using a combination of Spacers a...

Страница 59: ...C followed by work up with SiliaBond Carbonate and SiliaBond Carboxylic Acid to remove excess reagents and starting materials An SN Ar reaction allowed closure of the macrocycle once again followed by a purification step involving SiliaBond Carbonate Proc Natl Acad Sci USA 2011 108 6751 6756 Chemical Biology Platform Broad Institute Massachusetts United States Solution Phase Parallel Synthesis of ...

Страница 60: ...ography 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 We lead the way in offering innovative first rate UltraPure products Our automated manufacturing processes are continuously optimized to ensure high purity and a low percentage of fine particl...

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