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Daedalus RM User Manual

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User's Guide
RM Synthesizer
Version 1.02
Copyright ©2010
Daedalus Innovations LLC
Aston, Pennsylvania
United States

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Summary of Contents for Daedalus RM

  • Page 1 User’s Guide RM Synthesizer Version 1.02 Copyright ©2010 Daedalus Innovations LLC Aston, Pennsylvania United States...

  • Page 3: Table Of Contents

    TABLE OF CONTENTS LIST OF FIGURES ....................2   WARNINGS / INFORMATION ................... 3   ITEMS INCLUDED WITH THE RM SYNTHESIZER ..........4   ITEMS TO BE SUPPLIED BY THE END-USER ............5   INSTRUMENT SITE CONSIDERATIONS ..............6  ...

  • Page 4: List Of Figures

    Figure 3: Cleaning manifold assembly diagram ............8   Figure 4: Piston position during operation ..............10   Figure 5: RM Synthesizer Operational Description ..........12   Figure 6: RM Synthesizer Flow Diagram ..............13   Figure 7: Example valve actuation progression ............14  ...

  • Page 5: Warnings / Information

    Do not open the HP ALKANE TO BOOSTER valve on the RM Synthesizer if the reservoir is not filled with liquid CO .

  • Page 6: Items Included With The Rm Synthesizer

    ITEMS INCLUDED WITH THE RM SYNTHESIZER Below is the list of components that are supplied with the RM Synthesizer to facilitate setup. This list includes part numbers for possible replacement sources where appropriate. Quantity Description Source Elpac Power Systems 12V, 0.5A auto...

  • Page 7: Items To Be Supplied By The End-User

    Alkane gas cylinder: Typically the propane and ethane gas cylinders used with the RM Synthesizer do not have a regulator attached. The reason for this is the alkane is generally loaded into the cylinder at or near the liquefaction pressure. So in most cases the gas is withdrawn at maximum cylinder pressure hence no regulator is needed.

  • Page 8: Instrument Site Considerations

    The setup instructions below assume that the syringe pump to be used with the RM Synthesizer is the Daedalus Xtreme-10. The proposed arrangement of components is merely a guide.

  • Page 9: Connection Details

    could be turned orthogonal to the placement in the figure with a portion protruding outside the hood. If this configuration is selected, the Xtreme-10 should be placed on the left side of the hood with the inlet / outlet side facing to the right hand side. This places the internal tubing fully in the hood for optimal safety.

  • Page 10: Figure 3: Cleaning Manifold Assembly Diagram

    5) Connect a section of tubing to the WASTE port of the RM Synthesizer using a high pressure fitting. Assemble the Cheminert CFL-1N gland and sleeve on the free end. Feed this end through the small port of one of the three-port bottle caps until it is at the bottom of the bottle.
  • Page 11 6) Assemble the cleaning manifold according to the Figure 3 using the included parts and connect to the RM Synthesizer as indicated. 7) The NMR cell is connected to the OUTLET/INLET valve on the RM Synthesizer as indicated later in the instructions. This valve can also serve as the introduction point for deuterated alkane in situations where the syringe pump is not fully loaded with deuterated solvent.

  • Page 12: Theory Of Operation

    Rather than explain why other methods are not used, this discussion will focus on the what RM Synthesizer provides for this step. The liquid alkanes used in the preparation of...
  • Page 13 change in volume can be harnessed to rapidly move the piston when a reservoir at high pressure is allowed to relax to a lower pressure. This process is rapid, and the pressurizing fluid does not need to go through a transition from liquid to gas to deliver the needed force.

  • Page 16: Conventions Used In This Manual

    CONVENTIONS USED IN THIS MANUAL When describing operations of this device the identification of the valves involved will be made by listing the valve name that is stenciled on the instrument such as HP ALKANE or PISTON BOOSTER valve. The same method will be used to identify ports on the back of the instrument.
  • Page 17 syringe pump would then use protonated solvents to pressurize the sample. Due to the compressibility of ethane and propane, this will likely result is a sample that has 20-30% protonated solvent. INLET TO BOOSTER: This connects the CO INLET port directly to the gas booster.

  • Page 18: Back Panel Connections

    BACK PANEL CONNECTIONS Shown in Figure 8 are the ports used to connect the system to the external fluid sources required for operation of the RM Synthesizer. Figure 8: Back panel port connections HP ALKANE INLET: Connects to the outlet of the Xtreme-10 Syringe Pump. The tubing should be 1 kbar rated.

  • Page 19: Front Panel Control

    INLET so always have it connected or plugged to prevent discharging the nitrogen cylinder. CLEANING MANIFOLD: The outlet of the PEEK cross from Figure 3 should be connected to this port. Solvents from the cleaning manifold flow from this port to the mixing chamber.
  • Page 20 (3) Close the HP ALKANE TO BOOSTER and CO INLET TO BOOSTER valves. The gas booster is now filled with CO (4) Fill the syringe pump completely with liquid ethane. Follow the procedures in the Xtreme manual for refilling the pump. To extract liquid from the ethane cylinder it may be necessary to place the cylinder in warm water while filling the pump.

  • Page 21: The Mixing Chamber / Adding Reagents

    (8) Open the HP ALKANE TO BOOSTER and pump OUTLET valves to depressurize the gas booster. This will push out the ethane in the gas booster back into the syringe pump. Dependent on the pump fill factor and the initial CO head pressure, the pressure in the syringe pump will be around 1,500 psi.

  • Page 22: Figure 11: View Showing Internal Placement Of The Mixing Chamber Components

    Figure 11 shows the assembly diagram of the cell and the relative position of the components. The reagent plate serves two functions: The wall of the reagent plate stops the descent of the piston and prevents the stir bar from being crushed. Second, surfactants, especially liquid surfactants, can be weighed directly on this plate prior to inserting into the mixing chamber.

  • Page 23: Sealing The Mixing Chamber

    SEALING THE MIXING CHAMBER The high pressure seal is provided by the o-ring component P/N MCCS. This seal provides both a static containment seal during the sample mixing as well as a dynamic seal when the piston is driven down during the sample transfer step. This combination of forces tends to degrade the seal such that it must be replaced after every sample.

  • Page 24: Protocol For Making Samples

    (4) Tighten the four screws in a star pattern using a 3/16” hex driver in the pattern shown in the Figure 12. Once tightened, close the OUTLET / INLET valve. At this time it is recommended that all valves be checked to make sure they are closed, especially those that were actuated in the previous sample preparation process.
  • Page 25 Continue stepping up the pressure in small increments of 250 psi while continuing to observe the mixing process as noted by the cloudy nature of the sample. (6) Around 3,500 – 4,000 psi the sample should become noticeably more clear. At this point the experience of the user becomes important.

  • Page 26: Figure 13: Increasing The Sample Chamber Pressure Using The Piston

    all valves are closed, and open the VENT PISTON valves to release the pressure. Close the valve after venting is complete. ii,vii iii,vii Figure 13: Increasing the sample chamber pressure using the piston (7) Once the sample has been encapsulated it is recommended the internal sample pressure be increased by an additional 250 psi to account for potential pressure loss from the reverse micelle NMR cell over time.

  • Page 27: Transferring Samples From The Mixing Chamber To The Nmr Cell

    TRANSFERRING SAMPLES FROM THE MIXING CHAMBER TO THE NMR CELL With the sample now over pressurized to expand to fill the NMR cell internal volume, what remains is to apply sufficient pressure to the piston such that the sample is displaced from the mixing chamber into the NMR cell when the OUTLET / INLET valve is opened.

  • Page 28: Cleaning The Mixing Chamber

    (8) Be sure to clean the mixing chamber after each sample. CLEANING THE MIXING CHAMBER The RM Synthesizer is shipped with three low pressure glass reservoirs that can be filled with solvents for cleaning the mixing chamber and associated tubing after sample preparation.
  • Page 29 (1) Open the VENT PISTON valve to release the high pressure CO gas to the WASTE port. The remaining ethane in the mixing chamber will now push the piston back to the retracted position. (2) Open the WASTE valve to vent the sample to the WASTE port. Close the valve after the sample is vented.

  • Page 30: Resetting The System For The Next Sample

    (8) Go back to step (3) and repeat for each solvent in the list. (9) After cleaning the chamber, the cell cap can be removed. A screw from the cap can be threaded into the piston to remove it from the chamber (Figure 12). The seal (MCCS) should be removed and discarded.

  • Page 31: Tips

    . This method can be adapted to the user’s needs and time constraints. TIPS The following list contains some tips for operation of the RM Synthesizer some of which were contained in the text of this manual. It also contains tips that will hopefully help in making successful reverse micelle samples in ethane.
  • Page 32  No matter how good the seals, the system will leak over time. If the system will not be used for several weeks it is good idea to retract any deuterated solvents from the RM Synthesizer, into the syringe pump, and then push that fluid back into the alkane cylinder.

  • Page 33: Calibrating The System

     The encapsulation pressure is dependent on the dielectric constant of the medium. The elevated pressure is required to raise the dielectric of ethane to match the dielectric of the surfactant.  The encapsulation pressure can be lowered through the use of additives. This serves to increase the dielectric constant of the bulk solvent.

  • Page 34: Replacing The Window Seals

    (3) Open the WASTE valve to vent the alkane. This will purge the mixing chamber of air. (4) Change the setpoint on the syringe pump to 1,000 psi, and let it stabilize. (5) Note the current volume on the syringe pump, and open the HP ALKANE valve just enough to fill the chamber.

  • Page 35: Figure 16: Replacing The Mixing Chamber Windows

    filling the chamber with ethanol, pressurizing with the piston, and monitoring for leaks. Do not change the seals unless necessary. To remove: Figure 16: Replacing the mixing chamber windows (A) remove the four face plate screws. (B) Using a small L-shape hex wrench or equivalent, push out the plug from the inside.

  • Page 36: Figure 18: Reinserting The Window Plug

    Wet the seal with ethanol, and reinsert the assembled plug into the chamber wall (Figure 18). Figure 18: Reinserting the window plug Reattach the face plate using the four socket cap screws and incrementally tighten the screws using the pattern shown in Figure 19. This will better distribute the force on the window seal.

  • Page 37: Figure 20: Removing The Light Housing

    Figure 20: Removing the light housing (This section is intentionally blank)

  • Page 38: Specifications

    2006/95/EC. The standard used was EN 61010-1:2001 for electrical equipment for measurement, control, and laboratory use, Part 1: General requirements. Documentation can be provided by contacting in writing: Daedalus Innovations LLC 200 Racoosin Drive, Suite 106 Aston, PA 19014 United States.

  • Page 40: Further Information

    Technical support also obtained emailing questions support@daedalusinnovations.com, or contacting Daedalus directly at 610-358- 4728. Other correspondence can be directed to: Daedalus Innovations, LLC 200 Racoosin Drive, Suite 106 Aston, PA 19014...

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