Daedalus RM User Manual Download Page 31

 

29

 
(2) Change the setpoint on the syringe pump to 1,700 psi and start the pump 
running.  The high pressure CO

2

 fluid in the reservoir will now push the separator 

piston back towards the fully reset position.  Since some fluid was used during the 
sample preparation process it should not be expected to complete the full 
displacement.   
 
(3) With the pressure in both the reservoir and syringe pump below 1,800 psi the 

CO

2

 INLET TO BOOSTER 

valve can be opened to allow fluid from the gas cylinder 

to recharge the booster.  Once this valve is opened any excess alkane remaining will 
be forced back into the syringe pump, and a temporary pressure increase should be 
displayed by the syringe pump until it starts to readjust to the 1,700 psi setpoint.  
This process can take a few moments since the pressure differential is small. 
 
(4) Once the syringe pump is stable at 1,700 psi it can be assumed the separator 
has been fully reset since the applied 1,800 psi CO

2

 pressure is no longer 

influencing the syringe pump reading.  

Close

 the 

CO

2

 INLET TO BOOSTER 

the 

HP 

ALKANE TO BOOSTER 

valves.  The syringe pump 

OUTLET

 valve can be 

closed

 

as well. 
 
(5)  The system is now reset and ready for the next sample preparation. 
 
The primary goal of this protocol is to assure the gas booster reservoir is fully 
recharged with CO

2

.  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.  It is by no 
means exhaustive.   
 

  After the first few uses of an ethane or propane cylinder, the outlet pressure 

will likely be below the liquefaction pressure.  Placing the tank in warm water 
can help deliver liquid alkane from the cylinder. 

 

  Propane may not start to fill the mixing chamber until the pressure reaches 

300 psi.  The mixing chamber can be chilled to help condense propane, but it 
is by no means necessary to make it work. 
 

Summary of Contents for RM

Page 1: ...User s Guide RM Synthesizer Version 1 02 Copyright 2010 Daedalus Innovations LLC Aston Pennsylvania United States...

Page 2: ......

Page 3: ...4 VALVE DESCRIPTIONS 14 BACK PANEL CONNECTIONS 16 FRONT PANEL CONTROL 17 PREPARING THE INSTRUMENT FOR USE 17 THE MIXING CHAMBER ADDING REAGENTS 19 SEALING THE MIXING CHAMBER 21 PROTOCOL FOR MAKING SAM...

Page 4: ...e and main seal MCCS 19 Figure 11 View showing internal placement of the mixing chamber components 20 Figure 12 Progression of steps for assembling and sealing the mixing chamber prior to sample prepa...

Page 5: ...good practice to retract the gases from the RM Synthesizer back into the syringe pump and then push it back into the gas cylinder The MCCS seal is single use only Reuse of the seal or undertaking mult...

Page 6: ...P N 5557 20 4 PTFE 3 hole GL 45 caps VICI P N JR 9000 0001 1 PEEK Cross w fittings 28 threads VICI P N CXMPK 3 packs Cheminert glands and collars 28 threads 5 pack VICI P N CFL 1N 1 PEEK plug 28 thre...

Page 7: ...o exit as a liquid This requires the tank be equipped with an eductor or siphon tube so liquid CO2 will be drawn from the bottom of the tank High purity is not required For customers outside North Ame...

Page 8: ...ther configurations are possible and may be necessary depending on the space available It is important to stress the necessity of using the equipment in a ventilated space for the safety of the user T...

Page 9: ...nnected using the included 1 16 stainless steel tubing the high pressure 15 AM1 glands and 15 2A1 sleeves These steps should be followed when making a high pressure connection i Deburr the end of the...

Page 10: ...t on the RM Synthesizer to the N2 gas cylinder regulator 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 sle...

Page 11: ...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 alka...

Page 12: ...cycles to bring the pressure of the gas up to the level required Nitrogen is one of the best candidates However for certain applications the pressure required for the transfer step increases the dens...

Page 13: ...mp A separator piston in the reservoir keeps the fluids apart Once the transfer steps are performed the CO2 fluid can be used to push any deuterated alkane out of the reservoir keeping the losses to a...

Page 14: ...12 Figure 5 RM Synthesizer Operational Description...

Page 15: ...13 Figure 6 RM Synthesizer Flow Diagram...

Page 16: ...er to the sample tube perform the following steps diagramed in Figure 7 i Open the OUTLET INLET valve wait for two seconds ii Close the PISTON BOOSTER valve iii Open the HP ALKANE valve to equalize th...

Page 17: ...gas booster to the piston contained in the mixing chamber cap This can be used both to change the internal pressure of the mixing chamber without adding additional alkane to the sample as well as mor...

Page 18: ...should be anchored so it does not break loose when high pressure gas is vented CO2 INLET This is the high pressure carbon dioxide inlet Standard CO2 cylinders are not able to deliver liquid CO2 Instea...

Page 19: ...ep air circulating inside the instrument LAMP This knob controls the intensity of the light source illuminating the mixing chamber MIX This knob controls the sample stirring speed PREPARING THE INSTRU...

Page 20: ...is optional and does not need to be performed for routine operation of the instrument However this operation might be useful if a higher starting pressure is desired or if the time between syringe pu...

Page 21: ...ed There are slight variations between cells so an exact measurement should be obtained using the syringe pump see CALIBRATING THE SYSTEM Of this volume approximately 1 1 ml can be displaced by the pi...

Page 22: ...e should be placed at the bottom of the mixing chamber Make certain the WASTE valve is closed prior to adding reagents to prevent the reagents from being forced out through this port in subsequent ste...

Page 23: ...ng chamber for the high pressure work 1 Insert the o ring seal MCCS into the large chamber O D Push it down as far as it will go 2 Open the OUTLET INLET valve and push the piston to just slightly past...

Page 24: ...n free water stock with bromophenol blue added The visual indicator will help the user learn the tricks and visual markers that are apparent as the pressure on the sample is increased ultimately to th...

Page 25: ...tion since this would have negative consequences on the sample viscosity as well as the pressure could not be subsequently reduced as this would draw sample out of the chamber However the pressure on...

Page 26: ...be over pressurized to compress more molecules of ethane into the chamber such that once the transfer is initiated the sample will expand to fully fill the NMR tube The over pressurization required i...

Page 27: ...is included in the over pressurizing ratio Connect this tubing between the NMR cell and the OUTLET INLET valve 2 Open the PISTON BOOSTER and HP ALKANE TO BOOSTER valves Be sure the HP ALKANE valve is...

Page 28: ...w pressure glass reservoirs that can be filled with solvents for cleaning the mixing chamber and associated tubing after sample preparation Typically the solvents are water ethanol and dichloromethane...

Page 29: ...ly when the cell is opened to air however trace dichloromethane will not cause problems for reverse micelle formation For each cleaning solvent 3 Open the CLEANING MANIFOLD valve and open the appropri...

Page 30: ...roper position for the next sample This method can be used to confirm that the separator piston has been moved to the fully reset position At this point the reservoir pressure and syringe pump pressur...

Page 31: ...t since the applied 1 800 psi CO2 pressure is no longer influencing the syringe pump reading Close the CO2 INLET TO BOOSTER the HP ALKANE TO BOOSTER valves The syringe pump OUTLET valve can be closed...

Page 32: ...ize the mixing chamber to the encapsulation pressure or the new pressure desired Open the NMR cell valve and let the system equilibrate to the new pressure Close the NMR cell valve and the OUTLET INLE...

Page 33: ...5 should be considered for proteins larger than 40 kDa At this size the protein is dominating the size of the particle so the excess water has less impact Ethane can support much higher water loadings...

Page 34: ...000 psi setpoint 8 After the syringe pump has again stabilized note the new volume reading The difference between this volume and the volume in step 6 is the volume the piston can displace for the sam...

Page 35: ...n the recess of the plug Then place the o ring seal around the window as shown in Figure 17 Figure 16 Replacing the mixing chamber windows A remove the four face plate screws B Using a small L shape h...

Page 36: ...s using the pattern shown in Figure 19 This will better distribute the force on the window seal To replace the backside window first remove the lamp housing by unscrewing the power plug at the base an...

Page 37: ...35 This section is intentionally blank Figure 20 Removing the light housing...

Page 38: ...and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause harmful interference to radio communications Operation of this equipment in a r...

Page 39: ...37 Figure 21 Internal control board schematic...

Page 40: ...novations com in the support section for more recent versions of this document Technical support can also be obtained by emailing questions to support daedalusinnovations com or contacting Daedalus di...

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