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Biotage

®

Flash 75/150

User Manual

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Содержание Flash 150

Страница 1: ...Biotage Flash 75 150 User Manual ...

Страница 2: ...eservoir 14 Insert a Flash Cartridge 15 Pressurize the Radial Compression Module and the Solvent Reservoir 15 Equilibrate the Cartridge 16 Load Sample and Collect Fractions 18 Refill the Solvent Reservoir 18 Empty the Solvent Reservoir 18 Depressurize the Radial Compression Module and Remove the Used Cartridge 19 Clean the Sample Injection Module Biotage SIM 20 Troubleshooting 20 AM 190 Manifold 2...

Страница 3: ...he concerns of using glassware under pressure by utilizing durable polyethylene cartridges that are prepacked and completely self contained eliminating user exposure to silica dust HP API or any contaminants left after a separation Figure 1 Biotage patented radial compression technology improves flash separation performance and increases separation speed Distribution plate only Flash 75 O ring 10 ...

Страница 4: ...ash 150 and a red pressure indicator that sticks out when there is more than 20 psi 1 4 bar of inert gas pressure inside the radial compression module see Figure 2 Figure 2 The pressure indicator sticks out when the pressure inside the radial compression module is more than 20 psi 1 4 bar Figure 3 Safety relief valve Viton O ring Anodized aluminum barrel Pressure indicator Radial compression inert...

Страница 5: ...ve labeled MV 03 for turning the flow of compressed inert gas to the SIM on or off see Table 2 with an instant tight fitting for attaching tubing H2 I A valve labeled MV 02 for turning the flow of compressed inert gas to the solvent reservoir on or off see Table 2 with an instant tight fitting for attaching tubing I2 Valve Positions Valve Off Vent On Pressurize MV 01 PRR 01 BIOTAGE FLASH 75 150 CH...

Страница 6: ...wo of each type see Sanitary Gaskets below one chain clamp P N 01520 25 top frits P N FTF 0225 25 bottom frits with sealing rings P N FBS 1025 and one frit insertion tool P N 01596 for SIM 500 and 1000 and P N 03339 for SIM 2000 Figure 6 Three way valve Solvent flow Inert gas Sanitary clamp Frit holder 316 stainless steel tube Pour in liquids oils or coated samples To the radial compression module...

Страница 7: ... mm of 1 8 O D CLEAR PTFE tubing P N 00088 and one 1 six foot length 1830 mm of 1 4 O D CLEAR PTFE tubing P N 00089 Flash 150 one 1 twelve foot length 3658 mm of 1 4 O D CLEAR PTFE tubing P N 00089 Two 2 spare O rings for the radial compression module P N 00778 for Flash 75 and P N 01420 for Flash 150 One 1 two part inert gas supply fitting a 3 8 NPT reducing bushing with a 1 4 M NPT attached to a...

Страница 8: ...ropanol isopropanol IPA Formic acid methanoic acid HCOOH Acetic acid Ethanoic acid HOAc AcOH Deionized water H2O Trifluoroacetic acid TFA max 5 by volume n Heptane Piperidine pip Pyridine pyr Ammonia NH3 conc 23 27 by weight tert Butyl methyl ether TBME Diethyl ether 10 mM phosphate buffered saline pH 7 4 50 mM phosphate citrate buffer pH 5 0 Boric acid NaOH KCl buffer pH 11 Note The sample inject...

Страница 9: ...ding over the system for service it should be emptied of all liquid and cleaned from harmful residues It is the responsibility of the customer to inform Biotage 1 Point Support representatives if the system has been used with hazardous biological radioactive or toxic samples and or solvents prior to any service being performed If returning equipment to Biotage this should be done in accordance wit...

Страница 10: ...promised The system must not be operated unattended Never operate the system if damaged The system is operated using pressurized inert gas Ensure that all seals are properly mounted and that all clamps are properly closed before introducing pressurized gas into the system Confirm that the upper V band clamp is tight before compressing the radial compression module Only hand tighten the clamp to a ...

Страница 11: ... to the fume hood s mounting bars using mounting clamps not supplied 5 If using a Flash 150 radial compression module roll the cart with the module into a walk in fume hood Set Up the AM 190 Manifold Warning The AM 190 manifold must be mounted horizontally so that the water trap can function correctly The outlet of the safety relief valve must be directed away from the operator 1 Remove the AM 190...

Страница 12: ...ir is closed c The three valves on the AM 190 manifold are set to their off vent positions see Table 2 on page 3 2 Install a pressure regulator set to a maximum of 125 psi 8 6 bar to your inert gas supply 3 Install the brass fitting supplied with the start up kit the two part assembly with a 3 8 NPT reducing bushing and a 1 4 NPT instant tight tubing connector If using an inert gas supply in the f...

Страница 13: ... PRR 02 MV 01 PG 01 PG 02 MV 03 MV 02 N2 N2 N2 A B A C Inert gas supply B D E Schematics of a system ready for use when equilibrating the system and loading liquid sample left and when loading solid sample right A AM 190 manifold B sample injection module SIM C solvent reservoir D radial compression module and E fraction collection vessel Yellow tube pressurized inert gas inlet green tube inert ga...

Страница 14: ...is grounded before operating the system 2 Connect the next alligator clip item 2 in Figure 16 to the on off valve on the top of the solvent reservoir at the point where the metal tubing connector is located 3 Connect the next alligator clip item 3 in Figure 16 to the three way valve on the top of the sample injection module at the point where the metal tubing connector is located 4 Connect the nex...

Страница 15: ...CHROMATOGRAPHY AM 190 MANIFOLD PRR 02 MV 01 PG 01 PG 02 MV 03 MV 02 N2 N2 N2 A B System grounding schematic Note that all the alligator clips must be connected to metal fittings objects not to the plastic tubing 1 Connect to earth ground 2 3 4 5 6 7 10 8 9 ...

Страница 16: ... or at 500 pressure cycles whichever comes first Only use clamps and screws supplied by Biotage Confirm that the V band clamp is tight before compressing the radial compression module Only hand tighten the clamp to a maximum torque of 100 lbf in 11 3 Nm If the cartridge is not sealed properly replace the O ring and retry or contact Biotage 1 Point Support 1 Ensure that the three way valve on the r...

Страница 17: ...l compression pressure to 100 psi 6 9 bar by adjusting the PRR 01 regulator on the AM 190 manifold 7 Confirm that the cartridge is compressed the red pressure indicator on the front of the radial compression module sticks out see Figure 2 on page 2 8 Pressurize the solvent reservoir by turning the MV 03 valve on the AM 190 manifold to the on pressurize position see Table 2 on page 3 9 Set the equi...

Страница 18: ...Ensure that the MV 02 valve on the AM 190 manifold is set to its off vent position see Table 2 on page 3 and the two way valve on the solvent reservoir is closed 2 If loading a solid sample close the three way valve on the radial compression module and disconnect the solvent tube connected between the solvent reservoir and the radial compression module from the module and connect it to the SIM see...

Страница 19: ... compound will not elute in less than one column volume CV you may wish to collect the first 0 5 1 or 3 to 6 liters in a larger flask or carboy As you approach the point where your compound will elute use the smaller fraction collection vessels see the bullet list above to maximize your yield and purity Note Based on the predicted retention volume CP of the first compound the initial solvent volum...

Страница 20: ...isconnect the solvent tube from the radial compression module and insert it into a collection vessel of a suitable size 3 Turn the MV 03 valve on the AM 190 manifold to its on pressurize position see Table 2 on page 3 4 Lower the solvent pressure to 15 psi 1 bar 5 Take the necessary precautions to avoid exposure to harmful gases 6 While firmly holding down the solvent tube into the collection vess...

Страница 21: ...y is turned off and that the three valves on the AM 190 manifold are set to their off vent positions see Table 2 on page 3 3 Disconnect the two grounding clips attached to the SIM item 3 and 4 in Figure 16 on page 13 4 Loosen the clamp on the SIM and remove the top assembly clamp lid with the three way valve and sanitary gasket 5 Disconnect the SIM outlet tubing from the SIM 6 Remove the SIM from ...

Страница 22: ... and re apply PTFE tape and then re install using the appropriate wrench Top head assembly will not seat 1 Bottom head assembly is out of alignment 2 The cartridge is too long 1 Loosen the bottom head assembly re align to center and tighten the V band clamp 2 Contact Biotage see contact information on the back of this document or visit our website www biotage com Gas bubbles in the collection line...

Страница 23: ...the solvent pressure needs to be decreased Low viscosity solvents require lower inert gas pressure Sample Injection Module Biotage SIM Solvent Compatibility Check the solvent compatibility of the sanitary gasket used with the SIM by soaking it for one hour in your mobile phase Table 3 on page 4 summarizes the typical solvent compatibility If a gasket swells in use please let it dry out overnight i...

Страница 24: ...above 0 40 will elute too early i e less than 2 5 CVs whereas those with values much below 0 15 will consume excessive quantities of solvent The following sections address the two parameters used to optimize ΔCV solvent strength and solvent selectivity Rf CV Rf CV 0 90 1 10 0 45 2 20 0 85 1 17 0 40 2 50 0 80 1 25 0 35 2 80 0 75 1 33 0 30 3 33 0 70 1 40 0 25 4 00 0 65 1 54 0 20 5 00 0 60 1 65 0 15 ...

Страница 25: ...ne VII Hexane Heptane Iso Octane Table 7 Solvents commonly used for flash chromatography and their relative selectivity group In Figure 29 the Rf of the more polar component was changed by replacing ethyl acetate with dichloromethane and resulted in the upper i e less polar spot being essentially unchanged In some instances varying the polar solvent component can have a much more dramatic effect o...

Страница 26: ...h 75 and 150 prepacked cartridges In general the more difficult the separation i e a low ΔCV the less material can be loaded onto the cartridge for a successful high resolution separation Column Load ΔCV 0 1 1 9 Load ΔCV 2 0 3 9 Load ΔCV 4 Flash 75M 4 g 4 20 g 10 40 g Flash 75L 8 g 8 40 g 40 80 g Flash 150M 25 g 25 125 g 125 250 g Flash 150L 50 g 50 250 g 250 500 g Table 8 Predicting sample loads ...

Страница 27: ... the completion of a separation using one of the prepacked cartridges from Biotage you ll be able to evaluate the performance of the Biotage approach versus flash separations using traditional glass columns The workbook includes sections on Purification Goals Sample Compound Description Current Method TLC Method Optimization Prepacked Cartridge Data Run Analysis Fraction Collection Results Compari...

Страница 28: ... Workbook Flash Chromatography Workbook Chemist Account Department Address City State Zip Biotage Rep Date Purification Goals Sample Compound Description Current Method Column Size mm ID x mm long Silica grams Vendor Prep Time minutes Run Time minutes Solvent Used liters ...

Страница 29: ...LC Method Optimization Solvents Used Concentration Elution Calculations Rf CV Rf CV Rf CV Rf CV A A A A B B B B C C C C D D D D Rf CV 1 Rf Distance from the origin to the center of the spot Distance from the origin to the solvent front ...

Страница 30: ...ata Column Size mm ID x mm long grams of silica Sample Load grams in mL of Solvents Composition Volume liters Equilibrate Wash Elute Strip Flow Rate mL min Solvent Pressure Radial Compression Pressure Run Analysis Run Number Description Fraction Collection Fraction Volume liters Comments 1 2 3 4 5 6 7 ...

Страница 31: ... Fraction Collection continued 8 9 10 11 12 13 14 15 16 17 18 19 20 Results Fraction Solvent Front 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 20 Origin 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 Pools Recovered Wt ...

Страница 32: ...matography Workbook Comparison Analysis Flash Cartridge Glass Column Sample Size grams grams Flow Rate mL min mL min Preparation Time minutes minutes Purification Time minutes minutes Solvent Used liters liters Product Yield at Target Purity Summary Conclusions ...

Страница 33: ...www biotage com If you have problems downloading please contact your local Biotage representative Manufacturer Melrose Engineering Solutions for Biotage Sweden AB Contact Us Biotage Sweden AB Box 8 SE 751 03 Uppsala SWEDEN Visiting address Vimpelgatan 5 Phone 46 18 56 59 00 Fax 46 18 59 19 22 E mail info biotage com Website www biotage com Please contact your local Biotage representative See conta...

Страница 34: ...32 Biotage Flash 75 150 User Manual Biotage 2018 Notes Notes ...

Страница 35: ......

Страница 36: ... Part Number 02140 EN C 2018 Biotage All rights reserved No material may be reproduced or published without the written permission of Biotage Information in this document is subject to change without notice and does not represent any commitment from Biotage E OE A list of all trademarks owned by Biotage AB is available at www biotage com legal Other product and company names mentioned herein may b...

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