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Biotage Flash 75 User Manual

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Biotage
Flash 75/150
®
User Manual

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Summary of Contents for Biotage Flash 75

  • Page 1 Biotage Flash 75/150 ® User Manual...

  • Page 2: Table Of Contents

    Load Sample and Collect Fractions Refill the Solvent Reservoir Empty the Solvent Reservoir Depressurize the Radial Compression Module and Remove the Used Cartridge Clean the Sample Injection Module (Biotage SIM) ® Biotage Flash 75/150 User Manual | © Biotage 2018 ®...

  • Page 3: Introduction

    O-ring Radial compression inert gas supply Distribution plate (only Flash 75) 10 µm porosity frit External pressure Media applied Prepacked, disposable flash cartridge Compression barrel Figure 1. Biotage patented radial compression technology improves flash separation performance and increases separation speed.

  • Page 4: System Components

    . The components of the Flash 150 radial compression module. aluminum barrel with an instant-tight fitting for connection to The Flash 75 module has the same features but instead of being delivered the inert gas outlet on the AM-190 manifold (see page 3).

  • Page 5: Am-190 Manifold

    MV-03 MV-02 BIOTAGE FLASH 75/150 ® assembly is fitted with a three-way valve that connects to the CHROMATOGRAPHY MV-03 AM-190 MANIFOLD solvent reservoir and the outlet of the Biotage sample injection PG-01 PG-02 PRR-01 MV-01 PRR-02 MV-03 MV-02 module (Biotage SIM).

  • Page 6: Solvent Reservoir

    316 stainless steel tube with a sanitary clamp at the top and a compatibility information, see Table 3 below. stainless steel 1/8" (Flash 75) or 1/4" (Flash 150) tube fitting at the bottom. The top lid comes with a three-way valve. One port...

  • Page 7: Grounding Kit

    » One (1) user manual (P/N 02140). the Flash 75 system and a larger one for the Flash 150 system, For detailed information on how tubing and fittings are attached see Figure 9). For instructions on how to install the grounding and assembled, refer to the section “Installation”...

  • Page 8: Chemical Resistance

    Note: The sample injection module (SIM) is delivered with three types of sanitary gasket. Always check the gaskets' compatibility with the solvent or solvent mixture that you want to use. For more information, see “Sanitary Gaskets” on page 4. Biotage Flash 75/150 User Manual | © Biotage 2018 ®...

  • Page 9: Safety

    If returning equipment to Biotage, this should be done in accordance with the material return procedures supplied Biotage Flash 75 and Flash 150 systems are intended solely separately by Biotage. for purification. The systems must be operated in a laboratory environment with an ambient temperature between 4°C and...
  • Page 10 If the of any chemical or hazardous substance. system is used in a manner not specified by Biotage, the » Personnel working with or near the system must safety features of the system may be compromised.

  • Page 11: Installation

    4. Screw the lower half of the frit holder back in place. Finger- 4. If using a Flash 75 radial compression module: tight is normally adequate. a. Screw the two mounting rods into the mounting pads 5.

  • Page 12: Set Up The Solvent Reservoir

    Solvent Lines schematic in Figure 13). Warning Note: The Flash 75 start-up kit contains both 1/4" and 1/8" » clear PTFE tubing. The 1/8" tubing is to be used between the Always connect inert gas such as nitrogen to the gas inlet on the AM-190 manifold.
  • Page 13 Installation BIOTAGE FLASH 75/150 ® CHROMATOGRAPHY AM-190 MANIFOLD PG-01 PG-02 PRR-01 MV-01 PRR-02 MV-03 MV-02 Inert gas supply Figure 12 . Schematics of a system without the sample injection module (SIM). BIOTAGE FLASH 75/150 BIOTAGE FLASH 75/150 ® ® CHROMATOGRAPHY...

  • Page 14: Ground The System

    The one with the smaller nozzle and a tube with and a pair of fraction collection assemblies (see Figure 15). an outer diameter of 1/8" is for Flash 75 and the one with the larger nozzle and a tube with an outer diameter of 1/4" is for Flash 150;...
  • Page 15 Installation BIOTAGE FLASH 75/150 ® CHROMATOGRAPHY AM-190 MANIFOLD PG-01 PG-02 PRR-01 MV-01 PRR-02 MV-03 MV-02 Connect to earth ground Figure 16 . System grounding schematic. Note that all the alligator clips must be connected to metal fittings/objects, not to the plastic tubing.

  • Page 16: How To Use The System

    O-ring to seal the inert gas pressure within the barrel. Note that the V-band clamp should not be over-tightened. Maximum recommended tightening torque is 100 lbf-in (11.3 Nm). Biotage Flash 75/150 User Manual | © Biotage 2018 ®...

  • Page 17: Pressurize The Radial Compression Module And The Solvent Reservoir

    How to Use the System 6. Set the radial 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).

  • Page 18: Load Sample And Collect Fractions

    Figure 23. Inserting a frit into the SIM 2000 body using its frit insertion tool. Note that the insertion tool for SIM 500 and SIM 1000 does not have a handle. Biotage Flash 75/150 User Manual | © Biotage 2018 ®...
  • Page 19 For flash cartridges packed with KP-Sil silica, Biotage recommends a solvent flow rate between 100 and 250 mL/min for Flash 75 and between 400 and 1000 mL/min for Flash 150. Note: Ensure that the solvent pressure is at least 20 psi...

  • Page 20: Refill The Solvent Reservoir

    2. Disconnect the solvent tube from the radial compression module and insert it into a collection vessel of a suitable size. Biotage Flash 75/150 User Manual | © Biotage 2018 ®...

  • Page 21: Clean The Sample Injection Module

    13. Figure 26. The O-ring at the top of the radial compression barrel. 12. If the Flash 75/150 system is not used for a longer period of time or you want to change solvent before the next run, please empty the solvent tube that is connected to the solvent reservoir.

  • Page 22: Troubleshooting

    (5.5 to 6.9 bar). 2. Safety relief valve is defective. 2. Replace the safety relief valve (P/N 00790 for Flash 75 and P/N 02196 for Flash 150). 3. Safety relief valve is not properly 3. Remove and re-apply PTFE tape, and then re-install using the installed.

  • Page 23: Operation

    If less than 250 mL/min (Flash 75) or 1 L/min (Flash 150), replace the solvent tubing.

  • Page 24: Optimizing Flash Separations

    The following section is a summary of work completed by The following sections address the two parameters used to Biotage application chemists in an effort to reduce the amount optimize ΔCV; solvent strength and solvent selectivity. of trial and error that is typically associated with optimizing flash separations.

  • Page 25: Vary Solvent Selectivity To Maintain Values Between 0.15 And

    Optimizing Flash Separations Vary Solvent Selectivity to Maintain In Figure 29, the R of the more polar component was changed by replacing ethyl acetate with dichloromethane and resulted in Values Between 0.15 and 0.40 the upper (i.e. less polar) spot being essentially unchanged. Frequently, the R of one component can be changed relative In some instances, varying the polar solvent component can...

  • Page 26: The Relationship Between The Size Of A Column

    Load is Dependent on ΔCV Table 8 shows recommended sample loads for different length Flash 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.

  • Page 27: Flash Chromatography Workbook

    The Biotage Flash Chromatography Workbook has been designed to document the separation steps taken when using a Biotage Flash system to purify synthetic compounds. Upon 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.
  • Page 28 City: State: Zip: Biotage Rep: Date: Purification Goals Sample/Compound Description Current Method Column Size: mm ID mm long Silica: grams Vendor: Prep Time: minutes Run Time: minutes Solvent Used: liters Biotage Flash 75/150 User Manual | © Biotage 2018 ®...
  • Page 29 Flash Chromatography Workbook TLC Method Optimization Solvents Used: Concentration: Elution Calculations: Distance from the origin to the center of the spot CV= 1/R Distance from the origin to the solvent front...
  • Page 30 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 Biotage Flash 75/150 User Manual | © Biotage 2018 ®...
  • Page 31 Flash Chromatography Workbook Fraction Collection (continued) Results Fraction # Solvent Front Origin Pools: Recovered Wt.:...
  • Page 32 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 Biotage Flash 75/150 User Manual | © Biotage 2018 ®...

  • Page 33: General Information

    General Information General Information Price List and Ordering Information Please contact your Biotage distributor for the latest price and ordering information. Download User Documentation You can download the latest version of this document and other user documentation at www.biotage.com. If you have problems downloading, please contact your local Biotage representative.

  • Page 34: Notes

    Notes Notes Biotage Flash 75/150 User Manual | © Biotage 2018 ®...
  • Page 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.

This manual is also suitable for:

Flash 150

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