Daedalus RM Manuel utilisateur
User’s Guide
RM Synthesizer
Version 1.02
Copyright ©2010
Daedalus Innovations LLC
Aston, Pennsylvania
United States
1
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
CONNECTION DETAILS...........................................................................................7
THEORY OF OPERATION......................................................................................10
CONVENTIONS USED IN THIS MANUAL..............................................................14
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 SAMPLES...................................................................22
TRANSFERRING SAMPLES FROM THE MIXING CHAMBER TO THE NMR CELL
.................................................................................................................................25
CLEANING THE MIXING CHAMBER......................................................................26
RESETTING THE SYSTEM FOR THE NEXT SAMPLE..........................................28
TIPS.........................................................................................................................29
CALIBRATING THE SYSTEM.................................................................................31
REPLACING THE WINDOW SEALS.......................................................................32
SPECIFICATIONS...................................................................................................36
FURTHER INFORMATION......................................................................................38
2
LIST OF FIGURES
Figure 1: Possible bench-top setup............................................................................6
Figure 2: Possible fume hood setup...........................................................................7
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
Figure 8: Back panel port connections.....................................................................16
Figure 9: Front panel controls ..................................................................................17
Figure 10: Mixing chamber components: Poston, reagent plate, 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 preparation...............................................................................................21
Figure 13: Increasing the sample chamber pressure using the piston .....................24
Figure 14: Progression of valve actuation for the sample transfer steps..................26
Figure 15: Removing the piston ...............................................................................28
Figure 16: Replacing the mixing chamber windows .................................................33
Figure 17: Reassembly of the window plug..............................................................33
Figure 18: Reinserting the window plug ...................................................................34
Figure 19: Face plate tightening pattern...................................................................34
Figure 20: Removing the light housing.....................................................................35
Figure 21: Internal control board schematic.............................................................37
3
WARNINGS / INFORMATION
When the system contains alkane gas the system should be left turned
on since an internal fan constantly circulates the air in the instrument
case to prevent possible build-up of flammable gases.
The maximum pressure rating of this device is 1 kbar (14,500 psi).
Use of the system above this pressure can result in component failure
and possible injury to the user.
The system has been leak tested to the maximum pressure, however
when using gases, especially expensive deuterated reagents it is
prudent to not leave gases loaded in the system for extended periods
of time. It is 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
multiple displacement cycles of the piston at high pressure can cause
the seal to fragment leading to the loss of pressure tolerance or
causing the piston to be jammed in the cap or mixing chamber.
Do not open the HP ALKANE TO BOOSTER valve on the RM
Synthesizer if the reservoir is not filled with liquid CO2. This could
displace the internal separator of the gas booster to an unknown
position. Thus it is very important that the separator be reset to the
position closest to the alkane inlet on the gas booster (see Figure 6)
for proper function and transfer of samples to the NMR tube under
pressure.
4
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
1 Elpac Power Systems 12V, 0.5A auto
ranging power supply
1 AC power cord
30 ft. 1/16” O.D. x 0.03” I.D. stainless steel
tubing (1 – 10 ft. coil, 1 – 20 ft. coil) High Pressure Equipment
Company P/N 15-9A1-030
16 15,000 psi glands – ¼”-28 threads High Pressure Equipment
Company P/N 15-2AM1
16 15,000 psi sleeves High Pressure Equipment
Company P/N 15-2A1
4 1L Pressure resistant bottles Ace Glass P/N 5557-20
4 PTFE 3-hole GL-45 caps VICI P/N JR-9000-0001
1 PEEK Cross w/fittings – ¼”-28 threads VICI P/N CXMPK
3 packs Cheminert glands and collars – ¼”-28
threads; 5/pack VICI P/N CFL-1N
1 PEEK plug – ¼”-28 threads VICI P/N CPPK
3 PEEK shut-off valves – ¼”-28 threads Cole-Parmer P/N 02014-
00
1 PEEK check valve – ¼”-28 threads Cole-Parmer P/N 01355-
26
12 ft 1/16” O.D. polyethylene tubing Various sources
1 5/16” x 1/4” wrench
1 3/4” wrench
1 3/16” hex driver
200 MCCS mixing chamber cap seals
(primary) Daedalus
10 WS01 mixing chamber window seals
(spares) Daedalus
2 Stir bar
North America only
1 Nitrogen gas regulator; 150 psi max. out
1 Tescom Extreme Pressure Regulator;
6000 psi max in; 2,500 psi max out
1 0-3000 psi brass gauge
1 0-3000 psi brass gauge
1 CGA 320 brass nipple
1 CGA 320 brass nut
1 HiP 15-21AF1NMB adapter
1 HiP 15-21AF1NMC adapter
5
ITEMS TO BE SUPPLIED BY THE END-USER
Some additional tools may be required to complete the setup of the instrument.
Metal tubing cutter: A 1/16” metal tubing cutter and deburring tool will be
necessary to cut sections of tubing for making connections between the syringe
pump and RM Synthesizer and connections to the gas cylinders.
Teflon tape: This may be required when making attaching gas cylinder regulators.
The gas cylinder requirements are outlined below.
N2gas cylinder: Standard nitrogen gas cylinder. High purity is not necessary. For
customers outside of North America a suitable regulator capable of outlet pressures
of at least 120 psi – 150 psi (~8 bar - ~10 bar) is ideal.
CO2gas cylinder: Proper function of the RM Synthesizer requires that CO2be
delivered in liquid form. A standard CO2gas cylinder will NOT work for this purpose.
Many companies can apply 2,000 psi helium head pressure to a cylinder to allow the
CO2to exit as a liquid. This requires the tank be equipped with an eductor or siphon
tube so liquid CO2will be drawn from the bottom of the tank. High purity is not
required. For customers outside North America a regulator capable of outlet
pressures of at least 1,800 psi (124 bar) is preferred. Lower outlet pressures are
possible, but it should not drop below the liquefaction pressure of CO2 (~850psi @
RT).
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. However, it is likely an adapter will be required mate the 1/16” tubing from
the RM Synthesizer to the cylinder outlet. Due to the variance in cylinder types
Daedalus does not attempt to supply suitable adapters. Companies such as High
Pressure Equipment Company (www.highpressure.com) can help identify a proper
adapter once the outlet specifications for the particular alkane tank are identified.
6
INSTRUMENT SITE CONSIDERATIONS
The operation of this instrument involves the use of high pressure
carbon dioxide and flammable gases. Quantities of these gases are
vented from the system after sample preparation. For the safety of the
user this instrument should be setup in an exhaust hood or other
suitable ventilated environment.
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. Other 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.
The bench-top setup in Figure 1 assumes that the instrument in installed under an
appropriate exhaust hood. If that is not feasible, the instrument can be installed
inside a fume hood, however many fume hoods have a smaller depth than the length
of the Xtreme-10. This may require that the Xtreme-10 be placed towards the back
as shown in Figure 2. The Xtreme Controller would have to be placed outside the
hood, or mounted on top of the Xtreme Pump Box. Alternatively, the Xtreme-10
Figure 1: Possible bench-top setup
7
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. The Xtreme
Controller could then be placed on top of the Xtreme Pump Box. Not shown are
nitrogen and carbon dioxide cylinders which would be outside the fume hood.
CONNECTION DETAILS
Once the instruments have been positioned the equipment should be connected
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 tube section.
ii) Assemble the gland then sleeve onto the tube end.
iii) Insert the end of the tube into the fitting until it bottoms.
iv) Tighten the gland to 55 in·lb. A “bottoming out” or “dead stop” should be felt
when the connection is properly assembled.
Always use two wrenches when tightening fittings: one to tighten the
gland and one to prevent counter rotation of the fitting receptacle.
Failure to do so could break loose internal connections.
Make the following connections using high pressure tubing and fittings unless
otherwise specified:
Figure 2: Possible fume hood setup
8
1) Connect the OUTLET port of the Xtreme-10 to the HP ALKANE INLET port on
the back of the RM Synthesizer.
2) Connect the INLET port of the Xtreme-10 to the alkane gas cylinder.
3) Connect with high pressure the CO2INLET port on the RM Synthesizer to the
CO2gas cylinder regulator.
4) Connect the N2INLET port on the RM Synthesizer to the N2gas 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 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. Tighten the Cheminert gland to secure the line. The
remaining ports of this bottle cap should be left open to allow gases to vent.
Figure 3: Cleaning manifold assembly diagram
Table des matières
