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Flash Chromatography

Flash Chromatography. 150 & 300 ml/min Flash Pumps New 200 ml/min Binary Flash Pump. Flash 300. SPECIFICATIONS Flow Rate . . . . . .. . 0.1 – 300.0 ml/min Max. Pressure . . . . 200 p.s.i. Flow Accuracy . . . + 3% (10 – 250 ml/min) Dimensions . . . . . . 7.0" W x 12.0" D x 7.5" H

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Flash Chromatography

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  1. Flash Chromatography 150 & 300 ml/min Flash Pumps New 200 ml/min Binary Flash Pump

  2. Flash 300 SPECIFICATIONS • Flow Rate . . . . . .. . 0.1 – 300.0 ml/min • Max. Pressure . . . . 200 p.s.i. • Flow Accuracy . . . + 3% (10 – 250 ml/min) • Dimensions . . . . . . 7.0" W x 12.0" D x 7.5" H • Weight . . . . . . . . . . 20 lbs

  3. Flash 300 – Performance Data

  4. Flash 300 Features • Dual-Head Design for High Flow & Low Pulsation • Ceramic Pistons and High Performance UHMW, HPLC-grade Seals • Ruby Ball / Sapphire Seat Check Valves • Universal Voltage Input: 90 – 260 VAC / 50 – 60 Hz • Constant Flow Performance with Varying Back Pressure • Accurate Flow Rate and No Loss of Prime with Hexane, Methylene Chloride and other Light Solvents • Combination Prime-Purge Valve / ”T” / Single-Port Outlet (1/8”) • Additional Outlet Check Valve to Prevent Backflow during Priming • All-Stainless Steel Fluid Path (unless otherwise indicated – pistons, check valves & seals) • Fluid Path Isolated from Electrical Components • Interactive Digital Keypad, RS-232 PC Control & Monitoring, Remote Run/Stop • Fine-Tune Flow Calibration Set-Up Function: 2% increments to ±10% at 300 ml/min • EZChrom Driver available

  5. Compatible with Gradient Flash • Use the SCU 470 for stand alone gradient • 600ml/min isocratic • 300ml/min gradients • VUV 14 or Model 500 detector optional

  6. Simplicity and Function Calibration Button Run / Stop Button Power Switch Pump Inlet / Outlet Check Valve Holders One Capsule per Holder Pump Inlet / Outlet Check Valve Holders One Capsule per Holder Inlet (flexible tubing provided) Prime-Purge Valve Check Valve to Prevent Back Flow During Priming

  7. Calibrate for Any Solvent

  8. Flash 150 Binary Pump • 2 pumps in one cabinet • 150 ml/min for gradient • 300 ml/min isocratic • 150 p.s.i. max • Low cost for the flow range • Allows use of larger columns than other Binary pumping system

  9. NEW Binary Flash 200 SPECIFICATIONS • # Pumps . . . . . .. .. 2 • Flow Rate . . . . . .. . 0.1 – 200.0 ml/min each pump • Max. Pressure . . . . 200 p.s.i. • Flow Accuracy . . . + 3% (10 – 200 ml/min) Dimensions . . . . . . 7.0" W x 12.0" D x 7.5" H • Weight . . . . . . . . . . 20 lbs

  10. Binary Flash 150 & 200 Features • Two Single-Head Pumps with Electronic Fast-Refill for Low Pulsation in a Compact Package • Ceramic Pistons and High Performance UHMW, HPLC-grade Seals • Ruby Ball / Sapphire Seat Check Valves • Universal Voltage Input: 90 – 260 VAC / 50 – 60 Hz • Constant Flow Performance with Varying Back Pressure • Accurate Flow Rate and No Loss of Prime with Hexane, Methylene Chloride and other Light Solvents • Combination Prime-Purge Valve / ”T” / Single-Port Outlet (1/8”) • Additional Outlet Check Valve to Prevent Backflow during Priming • All-Stainless Steel Fluid Path (unless otherwise indicated – pistons, check valves & seals) • Fluid Path Isolated from Electrical Components • Interactive Digital Keypad, RS-232 PC Control & Monitoring, Remote Run/Stop • Fine-Tune Flow Calibration Set-Up Function: 2% increments to ±10% at max flow • EZChrom Driver available

  11. Flash Chromatography Today Demands • Higher throughput • Higher purity requirements • More Compounds purified in less time • A wider variety of compound types to separate

  12. Organic Chemists Face the Following Challenges • Little time to develop chromatography • Minimal interaction with instrumentation • Low solubility of compounds in water • Aqueous solvents incompatible with the next reaction • Difficult to remove water and alcohol • Very familiar with TLC • no time to optimize separation conditions

  13. Organic Chemists Require • High quantities of material • High loads • Systems for samples soluble in NP solvents • Must deal with low solubility and high volumes • Ever increasing purity requirements • Disposable columns • Simple to use hardware

  14. Today's Synthetic Reality • Modern synthesis is a multi step process • Purification between steps increases purity and yield • Except in biological synthesis samples are not RP compatible • HPLC is too expensive and sophisticated for synthesis purification • Old style flash is not fast enough nor giving high enough purity

  15. Unique Problems with Flash • Sample Load • Sample Solubility • Incompatibility of sample solvent with purification method Let the Flash 150, 200 & 300 solve these problems

  16. Volume Load Effects • Compared to analytical chemistry • Chemists require high sample loading (10mg-100’s gram) • End goal may only be 10 mg but may require 50-100 grams of starting material • Sample solubility problems require the use of solvents that are strong (cause elution of product)

  17. 1.80 C 150 mg in 18 mL 1.00 AU 0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10 1.80 B 150 mg in 8 mL AU 1.00 0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10 1.80 A Desired product 1.00 AU 150 mg in 1 mL 0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10 Loading Volume and Band-Broadening • Same sample loaded with constant mass: • 150 mg load • Three different cartridges • Chromatogram A: • Loading volume equivalent to 3% of column void volume (36 mL) • Chromatogram B: • Loading volume equivalent to 22% column void volume • Chromatogram C: • Loading volume equivalent to 50% column void volume • High volume Loads destroy the separation Minutes

  18. A 2.886 B 3.753 C 6.123  p Large Volume Loads Reduce Resolution • Illustrates the effect of sample volume on separation of component B from A • Sample load volume, as a percentage of void volume (Load Vol./Void Vol.), was plotted vs. resolution • Resolution degrades when sample load increase to 20% of the column void volume • Keep load at <20% of column volume

  19. Flash 150, 200 & 300 Solution to Loading Problems • Allows bigger columns so sample can be less than 20% of column void

  20. Mass loaded (mg) 1600 1400 1200 1000 800 700 600 400 300 200 100 50 Desired component 120 100 80 mV 60 40 20 0 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 Minutes High Mass Loading Destroys Separation • Sample volume was kept constant • 2 mL in 80/20 acetonitrile-water • Effect of sample load increase shown: • As mass increases, peak fronts shift • Peak tails overlap as mass increases • Load determines Column Size required

  21. Impact of Sample Mass on Separation • Ratio between loading mass and amount of packing material, Sample Mass/Packing (%), is shown vs. retention behavior: • When loading mass increases over 1.5% of the packing material, peak asymmetry increase significantly • Retention shifts to front as loading mass increases • As loading mass increases, peak tails overlap (without shifting)

  22. 3.596 1.425 Solvent and Co-Elution Reduces Loading Co-elution A B • A detailed fraction analysis for an affected purification • Total sample load 120 mg for components A and B • Sample dissolved in 0.8 mL dichloromethane • 95:5 Hexane-Ethyl Acetate as eluting solvent • Fractions are collected: 1.3 mL/fraction • Fraction purity was analyzed using HPLC and plotted vs. fraction number

  23. Flash 150, 200 & 300 Advantage • Allows column size to be matched to load with out sacrificing time due to low flows

  24. Synthesis catch-22 Organic Synthesis Trends More products/day • Organic chemists’ face rapidly changing, conflicting needs • More Synthesis • Greater output • Higher synthesis purity • Greater synthesis yields • A synthesis catch-22 dilemma Higher product purity Increased product yields

  25. Flash 150, 200 & 300 Changes the Game • Bridges the flash to prep HPLC gap • Allows a new approach to flash based on: • Higher pressures • Gradient • More efficiency

  26. Effect of Particle Size on Efficiency • 13-20 micron particles give optimal prep efficiency

  27. Effect of Efficiency on Resolution • Must square the number of theoretical plates to double resolution • Loading reduces high plate column efficiency faster than lower plate columns

  28. Capacity K’ • Measured in column volume • Think in terms of column volume’s of retention • Solvent strength effects k’ • Gradient changes k’ with time from infinity to less than 1

  29. Factors Affecting Capacity • Surface Area • Porosity • Particle density • Size • Active coating coverage • Solvent strength

  30. Effect of Particle Size on Pressure • Doubling particle size reduces pressure by a factor of 4 at the same linear velocity • Flash 200 & 300 allow 16-20 micron particles to be used • =Higher efficiency in the same time with more surface area

  31. Flash 150, 200 & 300 Advantage • The 200psi pressure limit allows smaller particles and higher resolution • Capacity can be dramatically Improved • Beat the CATCH 22 by using the Flash 200 & 300 benefits

  32. Gradient Effects • Can further dramatically increase through put by allowing full use of the column for purification. • Can actually shorten separation time. • Can concentrate samples

  33. Flash 300 & 200 & 150 Advantage • Can use SCU470 for stand alone gradient control • High flow in isocratic mode = 600ml/min for 2 Flash 300 and 400ml/min for Flash 200 • Gradient is now reasonable for Flash Separations

  34. SSI Offers • Single channel systems • Increase capability at moderate costs • A series of pumps for flash chromatography • System capability

  35. Flash 150, 200 & 300 Summary • Allows bigger columns so sample can be less than 20% of column void • Allows column sized to be matched to load with out sacrificing time due to low flows • The 200psi pressure limit allows smaller particles and higher resolution • Allows gradients • Easy calibration for a wide variety of solvents • Simplicity of design for reliable performance

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