Home
Agilent 1260 Infinity Analytical SFC System
Contents
1. Using the Agilent 1260 Infinity SFC Control Module 5 Shutting Down the SFC System The manner of shutting down the SFC depends on the requirement for rapid equilibration of the system on the next startup and the duration of the shutdown If the system will be shut down for some time it is probably best to shut down all components including the DAD and column oven These components tend to take longer to reach their stable operating conditions than the other components in the system You should always shut down both the SFC control module and the binary pump if the system is to be idle for a long time Partial Shutdown Injuries from pressurized CO gt Setting the pump to STANDBY does not depressurize the system Do not attempt to loosen fittings or perform maintenance under these conditions Serious skin and eye injuries can occur as the result of sudden release of CO in the liquid or supercritical state Always wear gloves and eye protection when maintaining the module 1260 Infinity Analytical SFC System User Manual 101 5 102 Using the Agilent 1260 Infinity SFC Control Module Leaving the system pressurized If the system is to be shut down for less than two hours a partial pressurized shutdown is recommended Press the control buttons for example button 2 to switch the Agilent 1260 Infinity SFC Control Module and binary pump states to STANDBY In this case the system remains pres
2. Remote Figure 30 Autosampler Signal Cable Connections 0 Power off l Power on 1260 Infinity Analytical SFC System User Manual 69 3 70 Installing the G4309A Agilent 1260 Infinity SFC System Installing an Injection Program in the Method The injector program is delivered as part of the default setup but you can enter it manually if necessary Table 14 Agilent 1260 Infinity SFC Autosampler Injector Program Injection Injection Volume Injection Mode Time Stoptime Posttime High Throughput Autom Delay Vol Reduction Overlapped Injection Minimized Carry Over Needle Wash Wash Mode Wash Time Wash Location Repeat Injector Cleaning Injection Valve Cleaning Valve Switching Time 1 Bypass Time 2 Mainpass Bypass Time 3 Mainpass Bypass Time 4 Mainpass Bypass Valve Movements Auxiliary Draw Speed Eject Speed Draw Position 15 0 pL Injector Program No Limit Off Off disabled Off Wash in Flushport 10s Vial 10 1 times off off off off 100 pL min 100 pL min 0 0 mm 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Table 14 Agilent 1260 Infinity SFC Autosampler Injector Program Equilibration Time Sample Flush Out Factor Vial Well Bottom Sensing Store Temperature Injector program table Row SN oO on FP wor 8 9 10 11 12 13 14 Agilent Contact
3. Z 3 3 BCD 6 40 oO 4 4 BCD 4 10 s je 2 5 5 BCDO 1 fie e9 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 5V Low 1260 Infinity Analytical SFC System User Manual 129 8 Identifying Cables External Contact Cable c50 o o ol 10 6 15 41 One end of this cable provides a 15 pin plug to be connected to Agilent modules interface board The other end is for general purpose Agilent Module Interface Board to general purposes p n G1103 61611 Color Pin Agilent Signal Name module White 1 EXT 1 Brown 2 EXT 1 Green 3 EXT 2 Yellow 4 EXT 2 Grey 5 EXT 3 Pink 6 EXT 3 Blue 7 EXT 4 Red 8 EXT 4 Black 9 Not connected Violet 10 Not connected Grey pink 11 Not connected Red blue 12 Not connected White green 13 Not connected Brown green 14 Not connected White yellow 15 Not connected 130 1260 Infinity Analytical SFC System User Manual Identifying Cables 8 CAN LAN Cables Both ends of this cable provide a modular plug to be connected to Agilent modules CAN or LAN connectors CAN Cables p n Description 5181 1516 CAN cable Agilent module to module 0 5 m 5181 1519 CAN cable Agilent module to module 1 m LAN Cables p n Description 5023 0203 Cross over network cable shielded 3 m for point to point connection 5023 0202 Twisted pair network cable shielded 7 m for point to point connection 1260 Infinity Analytical SFC System User Man
4. Cancel 9 Press OK to accept the settings 10 Click OK in the Agilent ChemStation Instrument Configuration to apply all configurations Instrument Configuration Configurable Modules Selected Modules Ww wo Agilent 1100 1200 Series LC Ato Configuration z Vahe et BiePump 513124 DE4I516819 P CotumeCompatementChuster P CohsnnComp 1513160 LP00000011 a gt D Froita Epa 1511604 ILP00000020 x SFC FLD 613214 000E PP1000 Agilent 1120 CompactLt a SFC SFC Fuson AS E copac 1522884 Z Ack for configuration change ot ChemStation startup 1260 Infinity Analytical SFC System User Manual 83 4 Configuring the System Setting up the Method Setting up the Method 1 In the Agilent ChemStation the method parameters for all RC Net devices including SFC settings are combined into a single tabbed dialog box Setup Method 1290 Infinity TCC 33 Valve FLD 3 Instument Curves 84 1260 Infinity Analytical SFC System User Manual Configuring the System 4 Setting up the Method 2 The Instrument Curves tab shows all instrument curves monitor traces available for storing with the acquired data file Setup Method TB BiPunp SFC of 1250 nny TOC Vave FLD EX Irstument Curves 1260 Infinity Analytical SFC System User Manual 85 4 Configuring the System Status 1 To start Aurora SFC Status in Agilent ChemStation go to View gt Instrument Ac
5. Preventative maintenance intervals can vary based on the system use The intervals offered in this section are for systems with average use of approximately 30 hours per week Infrequently used systems may extend these intervals while heavily used systems may require more frequent preventative maintenance Most service can be performed directly by the user or in house maintenance technicians Daily Inspection and Maintenance V Verify that power and signal cables are firmly connected and not under strain V Inspect all user serviceable high pressure tubes and transfer lines for crimping or very tight bends Replace as necessary V Wipe up any visible liquid spills or condensation on or near the instrument V Verify that all covers are securely fastened to the frame V Inspect all reservoirs to ensure an adequate solvent supply V Prime the wash pump and modifier pumps Check that the purge valve reseals without leaking V Empty all waste containers V Check that the exhaust line is attached to a ventilation system and that the ventilation system is drawing V If an inlet step down regulator is used with a gas supply system check that the inlet pressure is between 40 and 70 bar V Check the integrity of the SFC Flow path that is that column flow cell etc have not been removed V With the system running visually inspect unions and tees for leaks Run diagnostic leak test for added sensitivity V Check CO air monitor if a
6. c Replace the check valves Wipe off any residual liquid from external non sealing surfaces with a soft cloth such as a microfiber towel Replacing the Piston Seal 1 Sonicate or soak the new seal in isopropanol for 15 min to clean and provide lubrication for installing Place the replacement seal on the rod shaped end of the seal insertion removal tool so that the spring is visible when the seal is fully seated on the tool Insert the tool into the pump head so that the open side of the seal enters first facing the high pressure cavity of the pump head Be careful to line up the seal with the cavity while inserting Withdraw the tool leaving the seal in the pump head When you look into the pump head cavity only the polymer portion of the seal should be visible 1260 Infinity Analytical SFC System User Manual Tools required CAUTION Maintenance and Repair 6 Replacing the Pump Head 1 Fill the pump head cavity about one third full with isopropyl alcohol 2 Wet the piston tip with a few drops of isopropyl alcohol Holding an absorbent towel beneath the pump head assembly line up the pump head and carefully slide it into place Be sure that the inlet valve is on the bottom and the outlet valve is on the top Do not force the pump head into place 4 Finger tighten both knurled nuts into place To tighten firmly alternately turn nuts 1 4 turn while gently wiggling the pump head to center it 5 Re attach the in
7. formed or adhered to could result in damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated condi tions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indi cated conditions are fully under stood and met 1260 Infinity Analytical SFC System User Manual In This Book In This Book This Manual discribes all about the Agilent 1260 SFC System 1 Introduction to Supercritical Fluid Chromatography SFC This chapter provides an overview of the history theory and benefits of SFC 2 Site Requirements and Specifications This chapter provides information on environmental requirements physical and performance specifications only for the G4309 Agilent 1260 Infinity Analytical SFC System 3 Installing the G4309A Agilent 1260 Infinity SFC System This chapter provides an overview of the installation and setup of the hardware and software 4 Configuring the System How to configure the Agilent 1260 Infinity SFC Analytical system and Agilent 1260 Infinity SFC Control Module in ChemStation 5 Using the Agilent 1260 Infinity SFC Control Module This chapter provides information and hints on the use of the SFC System 6 Maintenance and Repair In
8. 1260 Infinity Analytical SFC System User Manual 51 3 52 Installing the G4309A Agilent 1260 Infinity SFC System Hardware Installation Wash pump inlet assembly 1 8 Teflon Tubing 0 pe is N f y N J i a Bottle filter Figure 18 Connecting the wash pump inlet The outlet of the injector wash pump is connected to the metering device in the Agilent autosampler To plumb the outlet side of the injector wash pump locate the was pump transfer line with check valve and install it in the upper port of the injector wash pump Flow through the wash pump is in the upward direction The injection wash system will not function if the check valve is improperly installed An arrow embossed on the check valve body indicates the direction of flow verify that the check valve is firmly installed Connect the wash pump transfer line with the spring loaded check valve A union is provided on the other side of the of the wash pump transfer line Follow instructions below for priming the injector wash pump before connecting the union and the autosampler metering device 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Metering device Needle Wash pump transfer line Wash pump transfer line Union 10 32 Peek tubing Figure 19 Connecting the Wash Line and Check Valve Priming the Injector Wash Pump The wash pump is NOT self priming it must be filled with wash so
9. fully exposes the piston and retaining ring Remove the retaining ring by prying it out with a small blunt instrument or tweezers at the slot provided Grasp the metal base of the piston assembly so that you avoid exerting any side load on the sapphire rod and remove the piston from the slot in the carrier by sliding it up Grasp the metal base of the replacement piston assembly and insert it into the slot in the piston carrier until it bottoms in the slot Replace the retaining ring and spacer Reattach the spacer mounting screws If properly positioned the spacer should be pressed into the foam wall seal 10 Gently slide the chiller back onto the pump mounting posts and firmly press it onto the spacer If properly positioned the chiller heat exchanger should now be pressed into the foam wall seal 11 Replace the piston seal 12 Replace the pump head 13 Replace the vapor shield Replacing the CO Inlet Filter 1 2 Unscrew the filter closure from the filter housing Use a seal insertion removal tool or a non metallic object such as a wooden toothpick to remove the large seal that remains in the housing 3 Unscrew the old filter and remove the small seal from the filter closure Place one of the small seals included in the replacement element kit over one of the new filters from the kit Screw the new filter into the filter closure finger tight Place one of the large seals from the replacement kit on the filter c
10. similarly above a critical temperature gases cannot be converted to liquids Above both the critical pressure and temperature characterized by the critical point solvents are in the supercritical state Under these conditions the mobile phases exhibit gaseous as well as liquid like properties The major advantages of this state related to chromatography are improved diffusion characteristics and mass transfer and low viscosity which result in high separation efficiency and fast separation capability 1260 Infinity Analytical SFC System User Manual 9 1 Introduction to Supercritical Fluid Chromatography SFC Benefits of SFC 10 SFC is widely accepted for the analysis and separation of chiral compounds In addition it gains increasing acceptance as a complementary liquid based separation technique to HPLC for high throughput and high resolution analysis of complex mixtures This is due to the thermodynamic properties of supercritical fluids which can be exploited for high throughput and high efficiency In addition the mild thermal conditions also allow for the analysis of thermally labile compounds Typically analysis times and column re equilibration are decreased by a factor of 3 5 compared to standard HPLC With the increasing costs of organic solvents and the environmental awareness to minimize toxic waste production SFC is increasingly accepted as the green alternative to normal phase or reversed phase chromatography
11. usually filled with that solvent The sample displaces some or all of this solvent If the loop is too large too much strong solvent is injected regardless of whether the loop is filled with sample or wash solvent Peaks will be distorted and efficiency will degrade 15 2 Injection Volume Figure 33 Plot showing loss of efficiency with large injection volume If a large loop is used air bubbles can be used to displace the wash solvent Less Polar Sample Solvents Help Replacing the sample solvent with a much less polar solvent can allow injection of much larger volumes However the new solvent must be significantly less polar than the modifier used Replacing methanol with ethanol or even isopropanol has minimal effect Solvents such as chloroform or methylene chloride tend to cause significant focusing NO broadening but since they are chlorinated should probably be avoided 74 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Software Installation The software installation consists of the following steps 1 Install Agilent ChemStation for more details see Agilent ChemStation for LC and CE Systems Installation Manual Chapter Installing the Agilent ChemStation Initial Installation 2 Install SFC USB driver 3 Install the Driver Software see Installing Agilent 1260 Infinity SFC Control Module Driver Software on page 75 Installing Agilent 1260 Infinity
12. 400 bar Cell path length 10 mm Cell volume 13 uL 34 1260 Infinity Analytical SFC System User Manual Site Requirements and Specifications 2 G4303A SFC Autosampler Table8 Physical Specifications Type Specification Comments Weight 15 5 kg 34 2 Ibs Dimensions height x width x depth 200 x 345 x 440 mm 8 x 13 5 x 17 inches Line voltage 100 240 VAC 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 300 VA 200 W 683 BTU Maximum Ambient operating temperature 4 55 C 41 131 F Ambient non operating temperature 40 70 C 4 158 F Humidity lt 95 at 25 40 C 77 104 F Non condensing Operating altitude Up to 2000 m 6562 ft Non operating altitude Up to 4600 m 15091 ft For storing the module Safety standards IEC CSA UL Installation category Il Pollution degree 2 For indoor use only Table9 Performance Specifications Type Specification Number of samples 100 x 2 mL vials 30 x 6 mL vials Injection volume 5 uL for full loop injections 5 uL loop as default larger loops possible 10 pL 20 uL partial loop filling for smaller injection volumes Injection principle Fixed loop Injection precision lt 0 3 RSD for 5 pL Sample temperature control 4 40 C with sample thermostat Sample carryover 0 05 1260 Infinity Analytical SFC System User Manual 35 2 Site Requirements and Specifications G4302A Binary SFC Pump Table 10
13. G4225A an SFC Autosampler G4303A a thermostatted column compartment G1316C and either a DAD G1315C or MWD G1365C equipped with a high pressure SFC flow cell and the SFC control module G4301A The SFC control module redestills and preconditions the CO by boosting the pressure to just below the column head pressure relieving the HPLC SFC pump of any compression requirements This results in low detector noise and significantly higher sensitivity Therefore the Agilent HPLC SFC pump receives pre conditioned COs and acts only as metering device for the mobile phase flow and to form the gradient with the second pump head by adding the appropriate amount of modifier solvent Downstream of the detector the mobile phase is redirected back into the SFC control module to an integrated back pressure regulator that maintains the backpressure over the system The Agilent 1260 Infinity SFC system is completely controlled by Agilent ChemStation software The system diagram is shown below Input Tee Wash pump from detector BPR to ALS from wash solvent bottle lt lt to Agilent SFC pump aee Output Tee Figure 2 Agilent 1260 Infinity Analytical SFC System 12 1260 Infinity Analytical SFC System User Manual Introduction to Supercritical Fluid Chromatography SFC 1 The Agilent 1260 Infinity SFC Control Module G4301A The Agilent 1260 Infinity SFC Control Module is responsible for all tasks connected to
14. Physical Specifications Type Specification Comments Weight 15 5 kg 34 Ibs Dimensions height x width x depth 180 x 345 x 435 mm 7 x 13 5 x 17 inches Line voltage 100 240 VAC 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 220 VA 74 W 253 BTU Maximum Ambient operating temperature 0 55 C 32 131 F Ambient non operating temperature 40 70 C 4 158 F Humidity lt 95 at 25 40 C 77 104 F Non condensing Operating altitude Up to 2000 m 6562 ft Non operating altitude Up to 4600 m 15091 ft For storing the module Safety standards IEC CSA UL Installation category Il Pollution degree 2 For indoor use only For use with flow rates below 500 L min or for use without damper and mixer a vacuum degasser is required All specification measurements are done with degassed solvents Table 11 Performance Specifications Type Specification Number of co solvents 1 with SSV pump option 3 with external SSV 12 Precision of flow rate Same as G1312B 0 07 0 07 RSD or 0 02 min SD whatever is greater based on retention time at constant room temperature Precision of composition Same As G1312B lt 0 15 RSD or lt 0 04 min SD whatever is greater 36 1260 Infinity Analytical SFC System User Manual Site Requirements and Specifications 2 G1316C Thermostatted column compartment Table 12 Physical Specifications Type Specification Comm
15. User Manual Maintenance and Repair 6 Preparing for storage or shipping If the SFC control module needs to be stored in other than its operational location it is best to store it in the original factory packaging This packaging can also be used to reship the device to a secondary location If the original packaging is unavailable the unit should be stored upright and preferably covered in a plastic bag or wrap to prevent exposure to dust To prepare the unit for storage use the following procedure Follow the standard decontamination procedure Depressurize the SFC system completely Power off the unit Remove the front panel Disconnect the wash pump transfer line from the autosampler Drain the wash pump lines of fluid uy oO ol FF WH Coil the lines to fit in the SFC control module behind the removable front panel 8 Disconnect the booster pump transfer line from the binary pump at the pump inlet check valve 9 Disconnect the BPR return line from the detector 10 Coil both lines to fit inside the SFC control module behind the removable front panel 11 Replace the front panel 12 Disconnect the power cord and all signal cables from both ends of the connection 13 Store cables and cords in a large plastic zip lock bag 14 Cover the unit with a large plastic bag 15 If the original container is available place the unit with its left side down in the packaging Otherwise store the unit upright in the storage are
16. circuit pump is powered The STANDBY state can also be entered by selecting the Standby option in the control window by pressing the power button associated with the SFC icon of the GUI or by pressing Off in the ChemStation graphical user interface once while the system is running When the STANDBY state is entered from the OFF state the BPR must be homed Once this is accomplished the BPR drive is active but in a hold state 1260 Infinity Analytical SFC System User Manual 93 5 94 Using the Agilent 1260 Infinity SFC Control Module When the Agilent 1260 Infinity SFC Control Module is in the STANDBY state the two status lights flash alternately The STANDBY state remains active for up to three hours If no user initiated action is taken to change or renew the state within this time a timeout occurs and the processor automatically enters the OFF state The ON State The ON state is characterized as follows V The COs supply valve is open powered V The booster pump drive is powered and begins to pump CO to the pressure target V The BRP drive is powered and the BRP begins the process of regulating to its setpoint V The BRP heater is powered V The chiller is powered V The secondary cooling circuit pump is powered The ON state can also be entered by selecting the On option in the control window by pressing the power button associated with the SFC icon of the GUI or by pressing On in the ChemStation graphical
17. in the right side of the oven This zone is used to precondition the fluid to column temperature and provide thermal control of the column The left side block is plumbed with the effluent from the column The purpose of the left side block is to independently match the temperature of the mobile phase to the optimum temperature for the detector In order to achieve minimum noise it is important to use the optimum conditioning temperature prior to detection typically between 37 C and 40 C for G1315C Left heat exchanger adjusted to Right heat exchanger is used to optimise detector noise post column adjust temperature pre column This temperature adjustment has effects on selectivity Figure 15 Plumbing the Agilent 1290 Infinity Thermostatted column compartment 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Connecting the SFC Autosampler Agilent Autosamplers need to be converted for use with SFC If this has not already been done refer to the installation and upgrade section of the Autosampler compatibility kit for specific instructions from pump 2 y needle seat Sy 3 5 pe Q hN 6 i N i E s5 contained waste to column ey Figure 16 Plumbing the G4203A SFC Autosampler If the autosampler has been upgraded the plumbing connections can be made to the injection valve In the external loop operation of the autosampler all connections are made on
18. of the time and is only switched to position one Load or Bypass to load sample The inside of the tube and needle needle port and valve body are all nearly continuously washed with fresh mobile phase during the run ALS modification for SFC using the three groove rotor In SFC the two groove rotor is replaced with a three groove rotor and an external loop is added to the injection valve The needle port is directed to enter either the inlet of the external loop or to waste The waste port is directed to either the outlet of the loop or to the needle port The pump is directed to either the inlet of the sample loop or to the column The column is directed to either the outlet of the sample loop or to the pump The inlet of the metering device is no longer connected to the injection valve but is instead connected to an external wash pump The metering pump should always be completely filled with the wash solvent with no air bubbles Loading Position The first position pump to column needle port to loop inlet waste port to loop outlet corresponds to the HPLC two groove rotor load position The needle is used to withdraw sample from the sample vial and air from the compartment in exactly the same way as for HPLC The same metering device 1260 Infinity Analytical SFC System User Manual Introduction to Supercritical Fluid Chromatography SFC 1 is used and driven at the same speed with the same accuracy and precision
19. report missing or damaged parts to your local Agilent Technologies representative Connecting the Waste system to the SFC control module BPR Outlet The Agilent 1260 Infinity SFC Control Module has a waste bottle located outside of the cabinet It can be located anywhere easily accessible and visible within the range of the supplied tubing The waste bottle serves multiple purposes and collects liquid waste from multiple sources The primary purpose is to separate the gaseous and liquid waste from the outlet of the BPR system in such a manner that the gaseous waste can be appropriately vented outside of the lab environment The waste bottle has input and output ports located above any collected liquids The mixed stream enters the waste bottle and the gaseous stream exits from the spout Proper system operation requires adequate space in the waste bottle to allow gaseous exit It is the responsibility of the operator to ensure that the waste bottle is empty before beginning operation of the SFC control module and to monitor and empty the waste bottle as needed during usage This is not a warning 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Tubing Tygon 3 8 1 4 1D SFC control module Waste Line Vented Waste Line 1 16 inch teflon SFC control module Waste Bottle Figure 12 Installing the Waste Container WARNING Exposure to toxic substances gt The vapor ex
20. stack 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 The injector wash pump The wash pump is required only with autosamplers normally operated as broken loop autosamplers converted to external loop autosamplers The injector wash pump requires a source of wash solvent This wash solvent is used to prime the injector system to ensure proper operation while aspirating sample If the metering device in the autosampler is not filled with solvent it can cavitate and yield anything between poor area reproducibility to no peaks no actual injection The wash pump also washes the injection system needle interior needle seat injection valve and sample loop before and after each injection The injector wash pump is connected to a bottle filter supplied through the wash pump inlet line The wash pump inlet line is connected to the lower port on the injector wash pump located on the left side of the BPR drawer The other end should be connected to the bottle filter The filter can then be placed in a user supplied wash solvent bottle The wash solvent bottle can be left on the bench or placed in the 1200 Infinity Series solvent cabinet The wash pump is connected to the metering device syringe pump through a check valve intended to prevent siphoning The operation of the check valve should be verified to ensure it is not leaking because this can cause a loss of injection precision
21. this chapter only the SFC specific procedures are described For procedures similar to the Agilent module procedures please refer to the single module manuals G1312C G1329B G1316C G1315 65C G4225A 7 Parts for Maintenance This chapter provides information on parts for maintenance and repair 1260 Infinity Analytical SFC System User Manual 3 In This Book 8 Identifying Cables This chapter provides information on cables used with the Agilent 1200 Infinity Series modules 9 Appendix This chapter provides addition information on safety legal and web 4 1260 Infinity Analytical SFC System User Manual Contents Contents 1 Introduction to Supercritical Fluid Chromatography SFC 7 History of SFC 8 Theory of SFC 9 Benefits of SFC 10 Common flow path overview for packed column SFC instrumentation 11 The Agilent 1260 Infinity Analytical SFC System 12 2 Site Requirements and Specifications 23 Site Requirements 24 Specifications 28 3 Installing the G4309A Agilent 1260 Infinity SFC System 39 Hardware Installation 40 Software Installation 75 4 Configuring the System 79 Configuring SFC interface in ChemStation 80 Setting up the Method 84 Status 86 Control 87 Testing the System 88 5 Using the Agilent 1260 Infinity SFC Control Module 89 Powering up the Module 90 Power up Sequence and Operational Control States 91 Operational Control States 92 Controlling the Agilent 1260 Infinity SFC Control Module t
22. user interface When the Agilent 1260 Infinity SFC Control Module is in the ON state the top status light is continuously lit The bottom status light is lit when the system reaches a ready state indicating that backpressure and booster pump pressure are under control and stabilized within their control band Modules that start from the OFF state generally must first perform an initialization routine before moving to ON In the case of the Agilent 1260 Infinity SFC Control Module initialization causes the BPR first to home then move to a default initialization position The booster pump delays operation until the chiller passes below a threshold temperature value 1260 Infinity Analytical SFC System User Manual Using the Agilent 1260 Infinity SFC Control Module 5 Controlling the Agilent 1260 Infinity SFC Control Module through the Agilent ChemStation Exploring the module Graphical User Interface GUI x M Control C On Off C Standby I DePressurize Figure 34 Setting Control State 1260 Infinity Analytical SFC System User Manual 95 5 Using the Agilent 1260 Infinity SFC Control Module Controlling the Agilent 1260 Infinity SFC Control Module through the Agilent ChemStation Nozzle Pressure 100 bar Nozzle Temp 60 Hce as master no limit 1 00 min Figure 35 Editing the SFC control module Method Parameters Editable method parameters for the Agilent 1260 Infin
23. valve holder Danger of piston breakage gt Be careful not to break the piston when removing the pump head Twisting the pump head can cause the piston to break 6 Using the 3 16 hex drive carefully remove the two knurled nuts at the front of the pump head Carefully separate the pump head from the pump Move the pump head straight out from the pump and remove it from the piston Be careful not to break or damage the piston Also remove the seal from the piston if it did not stay in the pump head 1260 Infinity Analytical SFC System User Manual 111 112 Maintenance and Repair 8 Ifthe seal remains with the pump head insert the flanged end of the seal insertion removal tool into the seal cavity Tilt it slightly so that flange is under the seal and pull out the seal Inspecting and Cleaning the Pump Head 1 Visually inspect the piston seal cavity in the pump head Use magnification if necessary Remove any foreign material using a cotton swab or equivalent and avoid scratching the sealing surfaces Be sure no fibers from the cleaning swab remain in the components The pump head may be further cleaned as follows a Remove inlet and outlet check valves b Clean with 50 isopropanol in water in an ultrasonic bath for at least 30 min followed by rinsing for at least 10 min in 100 isopropanol Be sure that all particles loosened by the above procedures have been removed from the components before re assembly
24. 0 APG Remote ready start stop and shut down signals relay contact closure wash pump only 1260 Infinity Analytical SFC System User Manual 31 2 Site Requirements and Specifications Agilent 1260 Infinity System Unspecified Conditions Operating the instrumentation under conditions other than its intended use might result in a potential safety hazard or might damage the instrumentation gt Never operate your instrumentation under conditions other than those specified by the vendor 32 1260 Infinity Analytical SFC System User Manual Site Requirements and Specifications 2 G4225A Vacuum Degasser Table5 Physical Specifications Type Specification Comments Weight 5 kg 11 Ibs Dimensions height x width x depth 80 x 345 x 435 mm 3 1 x 13 5 x 17 inches Line voltage 100 240 VAC 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 30 VA 30 W 102 BTU Maximum Ambient operating temperature 0 55 C 32 131 F Ambient non operating temperature 40 70 C 4 158 F Humidity lt 95 at 25 40 C 77 104 F Non condensing Operating altitude Up to 2000 m 6562 ft Non operating altitude Up to 4600 m 15091 ft For storing the module Safety standards IEC CSA UL Installation category Il Pollution degree 2 For indoor use only 1260 Infinity Analytical SFC System User Manual 33 2 Site Requirements and Specifications G1315C D Diode Array Detector and M
25. 1200 1260 LC Option for SFC UHPLC in one system Yes Unattended operation Leak sensors diagnostic software features Agilent 1260 Infinity SFC Control Module Select the laboratory bench space before your system arrives Pay special attention to the total height requirements Avoid bench space with overhanging shelves Pay special attention to the total weight of the modules and solvents you have in addition to the Agilent 1260 Infinity SFC Control Module Make sure that your laboratory bench can support this weight im The Agilent 1260 Infinity SFC Control Module module is heavy gt Enlist the aid of a co worker to share the lifting load to avoid personal injury 28 1260 Infinity Analytical SFC System User Manual Site Requirements and Specifications 2 Table 1 Physical Specifications G4301A Type Specification Weight 26 kg 56 Ibs Dimensions height x width x depth Line voltage Line frequency Power consumption Operating temperature Non operating temperature Humidity Laboratory ventilation Exhaust vent capacity Operating altitude Non operating altitude Safety standards 60 cm x 26 cm x 48 cm 23 in x 10 in x 18 in 100 240 VAC 10 50 60 Hz 5 700 VA Max 15 30 C 40 70 C lt 95 at 40 C Non condensing minimum 6 air exchanges hr for lab air CO monitor recommended w alarm 5000 ppm gt 20 L min with sustained negative pressure up to 2000 m 6500 ft up to
26. 3 1 14 Introduction to Supercritical Fluid Chromatography SFC SFC Autosampler G4303A In SFC the complete solvent flow path needs to be pressurized under all conditions to avoid expansion of the supercritical fluid This excludes the use of a variable injection loop design that is generally used in other Agilent autosamplers Therefore the autosampler used in the Agilent 1260 Infinity analytical SFC system has been converted to a fixed loop injector containing a 5 uL sample loop The injection loop of the autosampler is installed between two ports of the 2 position 6 port injection valve The total delay volume of the injector is about 3 3 uL As with any fixed loop injector overfill of sample is necessary to inject 5 uL reproducibly To completely fill the sample loop an excess of sample is required This is about 3 loop volumes 15 uL of the installed loop of sample to achieve 95 of the maximum loop volume For smaller injection volumes the loop needs to be partially filled by sandwiching the sample between two air bubbles one on either side followed by a plug of modifier or other solvent behind the sample Default methods for full loop filling are provided and should be used as initial injection conditions The default methods are automatically loaded in ChemStation The recommended temperature setting on the left heat exchanger in order to achieve minimum noise is typically between 37 C and 40 C for G1315C or G1365C
27. 4600 m 14950 ft IEC EN CSA UL Installation Category Il Pollution Degree II For Indoor Use only The Agilent 1260 Infinity SFC Control Module is heavy approximately 26 kg or 56 lbs Enlist the aid of a co worker to share the lifting load in order to avoid possible injury It should be positioned on a sturdy bench capable of holding the total weight of the Agilent 1260 Infinity SFC Control Module plus the Agilent 1260 Infinity system 1260 Infinity Analytical SFC System User Manual 29 2 30 Site Requirements and Specifications Table 2 Chemical Specifications G4301A Type Specifications Inlet CO bulk purity Inlet CO phase Inlet CO supply pressure Inlet CO temperature Wash solvent Liquid coolant Coolant volume gt 99 99 vapor gt 99 999 liquid vapor from non dip tube high pressure cylinder liquid from commercial CO delivery system 40 70 bar 580 1000 psi 15 30 C HPLC grade alcohol 30 propylene glycol in deionized water proprietary antioxidants red dye added for safety lt 280 mL Table 3 Wetted Materials Specifications G4301A Type Specifications High pressure flow path Low pressure flow paths waste wash pump leak tray Vapor exhaust 300 and 400 series stainless steel PEEK carbon filled PEEK PTFE PTFE FEP CTFE UHMW PE ruby sapphire ceramic 316 stainless steel PEEK PTFE PTFE FEP CTFE CPE LDPE Tygon PVC Tygon
28. 9 5 Using the Agilent 1260 Infinity SFC Control Module Powering up the Module The Agilent 1260 Infinity SFC Control Module is powered on by pressing the top of the rocker type power switch located on the upper right rear of the module Once the rocker is pressed the module responds by entering its power up sequence The power button of the module must remain accessible at all times Never arrange equipment so that the switch cannot be accessed WARNING The power switch has to be reachable for emergency gt The power switch of the module must remain accessible at all times Never arrange equipment so that the switch cannot be accessed 90 1260 Infinity Analytical SFC System User Manual Using the Agilent 1260 Infinity SFC Control Module 5 Power up Sequence and Operational Control States When power is applied to the Agilent 1260 Infinity SFC Control Module a series of events is initiated The order of these events is designed to safely initialize and test individual component functionality The module power up sequence executes the following steps 1 Power is automatically applied to the processor and the two module fans 2 The processor initializes a Any temporary configuration or calibration data that has not been stored in flash memory is lost b A checksum validation is made of data stored in flash memory c A self test is run to test power supply voltage levels and sensor readings for in range values d Stored c
29. AN N p n _ e tf Agilent Technologies Notices Agilent Technologies Inc 2010 2012 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 64301 90001 Edition 12 2012 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn This product may be used as a com ponent of an in vitro diagnostic sys tem if the system is registered with the appropriate authorities and com plies with the relevant regulations Otherwise it is intended only for gen eral laboratory use Warranty The material contained in this docu ment is provided as is and is sub ject to being changed without notice in future editions Further to the max imum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or perfor mance of this document or of any information contained herein Shou
30. D MWD Carefully examine the inlet and outlet ports of the cells to ensure that flow is in the correct direction In the DAD MWD the outlet port is normally located below the inlet port on the connection block The inlet port of the DAD MWD flow cell enters the stationary portion of the handle This stationary bar acts as an initial thermal conditioning zone Normally this port has a male fitting The outlet port connects directly to the cylindrical portion of the flow cell Normally this connection has a female fitting iv f A V SY LP an M f Figure 13 DAD SFC Flowcell CAUTION Damage to the flowcell gt Verify that the cell installed in the detector is capable of the high pressures used in Supercritical Fluid Chromatography SFC Exposing a standard 1260 Infinity flow cell to high pressures will result in leakage or damage to the cell 46 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Hardware Installation Connecting the BPR to the 1260 Infinity stack Connect the Agilent 1260 Infinity SFC Control Module return transfer tube to the outlet block of the detector This tube can then be routed out the concave opening in the bottom of the detector behind the detector cover The return transfer tube should then be routed to the space between the 1260 Infinity stack and the Agilent 1260 Infinity SFC Control Module Move the tube upward between the units and throug
31. Hardware Installation 40 General Procedures 40 Installing Agilent 1260 Infinity SFC Control Module G4301A 43 Preparing the HPLC 62 Software Installation 75 Installing Agilent 1260 Infinity SFC Control Module Driver Software 75 This chapter provides an overview of the installation and setup of the hardware and software ott Agilent Technologies 39 3 Installing the G4309A Agilent 1260 Infinity SFC System Hardware Installation General Procedures Proper use of wrenches Some of the plumbing connections require a nut to be tightened onto a fitting There are often two sets of flats next to each other Attempting to tighten the nut without securing the other part of the fitting with a second wrench can result in loosening yet another connection upstream or downstream It is best practice to always hold the fitting with one wrench while tightening or loosening another connection D5 Figure 10 Proper tightening of Fittings 40 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Compression Swaged Fittings The fittings used in the Agilent 1260 Infinity SFC Control Module are Valco Fittings used in all Agilent modules are Swagelok Use the appropriate fitting as recommended by the equipment manufacturer The recommended tightening procedure to install new fittings is to tighten the nut finger tight then an additional 1 4 to 1 2 turn to seal In general previously swa
32. PVC Performance Specifications Table 4 Performance Specifications G4301A Type Specifications Hydraulic system Total hydraulic volume Single piston with proprietary motor control lt 5 mL pressure lt 70 bar lt 25 mL pressure up to 400 bar 1260 Infinity Analytical SFC System User Manual Site Requirements and Specifications 2 Table4 Performance Specifications G4301A Type Specifications Chiller system Back Pressure Regulation BPR system Chiller temperature Booster pump speed range Booster pump pressure range Pressure pulsation BPR thermal range BPR thermal precision BPR pressure range Backpressure accuracy Backpressure precision Backpressure thermal precision Control and data evaluation Analog in pressure monitoring Communications Thermoelectric cooling with secondary air liquid cooling circuit Low volume diaphragm type with proprietary drive control replaceable BPR head assy No recalibration required after head replacement 20 9 C 0 6000 steps sec average step rate 100 400 bar up to 5 mL min demand lt 2 amplitude at pump speed gt 300 steps sec and outlet pressure gt 100 bar 40 70 C 104 158 F 1 C 100 400 bar 1 0 5 bar 0 2 bar typical 1 C Agilent ChemStation for LC with SFC Control Module driver SFC Control Module Diagnostic Program 1 V FS one input range set by calibration to host pump USB 2
33. SFC Control Module Driver Software The driver is installed as an add on product for ChemStation The following screenshots show the installation steps It is important to select the ChemStation installation directory as destination path 1 Start the Sfc Fusion ChemStation Interface Setup Wizard if Sfc Fusion ChemStation Interface Welcome to the Sfc Fusion ChemStation Interface Setup Wizard AION A The installer will guide you through the steps required to install Sfc Fusion ChemStation Interface on your computer WARNING This computer program is protected by copyright law and international treaties Unauthorized duplication or distribution of this program or any portion of it may result in severe civil or criminal penalties and will be prosecuted to the maximum extent possible under the law 1260 Infinity Analytical SFC System User Manual 75 3 Installing the G4309A Agilent 1260 Infinity SFC System Software Installation 2 Select installation folder i8 Sfc Fusion ChemStation Interface Select Installation Folder 3 Confirm installation i Sfc Fusion ChemStation Interface Confirm Installation D 76 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System Software Installation 4 Install the Sfc Fusin ChemStation Interface if Sfc Fusion ChemStation Interface Installing Sfc Fusion ChemStation Interface i Sfc Fusion ChemStation Interface I
34. The needle is then positioned in the same needle port just as it is for HPLC External loop in To From pump waste External From loop out needle port To waste Figure 5 Loading position Full loop injections For full loop injections the amount of sample withdrawn is actually substantially larger than the volume of the loop This volume is normally two to three times greater than the sample loop s volume Most of this larger volume is pushed through the loop overfilling it The physical volume of the loop is primarily what determines the precision of the injection and the actual amount injected The accuracy of the metering device is of secondary importance Overfilling the loop guarantees that the sample is a midstream sample without the dilution found on the ends caused by the parabolic flow profile of the sample as it moves through the tubing Compared to the standard approach the external loop mode wastes sample when maximum precision is required However reproducibility can be identical in both cases Modifying the Agilent ALS for SFC adds an additional step when setting up injections The needle port and its connecting tubing have approximately 2 uL of dead volume after the needle and before the sample loop In HPLC two groove rotor this tube is flushed with mobile phase during injection In SFC this tube is no longer exposed to flowing mobile phase and any sample left in the tubing during injection will be lo
35. WD G1365C Table6 Physical Specifications Type Specification Comments Weight 11 5 kg 26 Ibs Dimensions height x width x depth 140 x 345 x 435 mm 5 5 x 13 5 x 17 inches Line voltage 100 240 VAC 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 160 VA 160 W 546 BTU Maximum Ambient operating temperature 0 55 C 32 131 F Ambient non operating temperature 40 70 C 4 158 F Humidity lt 95 at 25 40 C 77 104 F Non condensing Operating altitude Up to 2000 m 6562 ft Non operating altitude Up to 4600 m 15091 ft For storing the module Safety standards IEC CSA UL Installation category Il Pollution degree 2 For indoor use only ASTM Standard Practice for Testing Variable Wavelength Photometric Detectors Used in Liquid Chromatography Reference conditions cell path length 10 mm time constant 1 s equal to response time 2 s flow 1 mL min LC grade Methanol slit width 4 mm Linearity measured with caffeine at 265 mm Table7 Performance Specifications Type Specification Wave length range 190 950 nm Wavelenghth accuracy 1 nm Linearity range 2 0 AU at 265 nm Noise wet 0 05 mAU under SFC conditions at 254 nm 20 MetOH 80 CO at optimum preconditioning temperature setting typically between 37 C and 40 C for G1315C or G1365C 0 007 mAU under LC condition Drift 0 9 mAU h Data rate 80 Hz Cell pressure limit
36. a 16 If the HPLC will also be stored or shipped and will be reconfigured as an SFC system the upgrade components can remain in the system 17 If the two systems are to be permanently separated uninstall the check valves modifier purge valve 3 groove rotor and high pressure flow cell by reversing the installation procedures in Hardware Installation on page 40 Store the components along with the original software disc and any upgrades with the module 1260 Infinity Analytical SFC System User Manual 117 6 Maintenance and Repair General Maintenance procedures 118 1260 Infinity Analytical SFC System User Manual 7 1260 Infinity Analytical SFC System User Manual KP e e EEE ee 7 90 e Parts for Maintenance amp o e e J Agilent 1260 Infinity SFC Control Module Parts 120 Agilent Module Parts 121 This chapter provides information on parts for maintenance and repair a Agilent Technologies 119 7 Parts for Maintenance Agilent 1260 Infinity SFC Control Module Parts 120 p n G4301 60350 G4301 60260 G4301 60250 G4301 60140 G4301 60130 G4301 60210 G4301 60230 G4301 60120 G4301 60240 G4301 60241 G4301 60300 G4301 60310 G4301 60320 G4301 60150 G4301 60160 G4301 60560 G4301 60340 G4301 60330 0100 2606 G4301 00200 G4301 60220 G4301 60500 Description Tee Valco Booster Pump Head A5 Pump Seals 2pk Wash Pump Seal Kit Wash Pump Piston Assy Check Valve Cartridge 0 125 ball Chec
37. alibration and configuration data are downloaded to RAM e The event logbook is updated The booster pump drive is rotated to find its index pulse 3 4 Index pulses are tested for module fans and the coolant pump 5 The BPR is homed to its fully open depressurized position 6 If installed the wash pump is rotated to its index pulse At the completion of a successful power up sequence the processor places the module in the OFF operational state described in Operational Control States on page 92 If an error is encountered and unresolved after multiple attempts the module is placed into the ERROR state and a notation is stored in the event log 1260 Infinity Analytical SFC System User Manual 91 5 Using the Agilent 1260 Infinity SFC Control Module Operational Control States 92 The Agilent 1260 Infinity SFC Control Module has three defined operational control states OFF STANDBY and ON You control the three states by selecting the Control option from either the ChemStation SFC Fusion icon by pressing various icons of the ChemStation GUI or from the Aurora A5 Diagnostic Program status tab Some components of the Agilent 1260 Infinity SFC Control Module are not governed by the three described states but are continuously on These include V The processor Continuously records and transmits sensor data to the host control system Handles status and command requests from the host controller Monitors sensors for
38. crificial fitting Connections should be made to the less expensive component and repetitive removal and replacement to one of the more expensive fittings should be avoided 1260 Infinity Analytical SFC System User Manual 41 3 Installing the G4309A Agilent 1260 Infinity SFC System Hardware Installation Nut Compression fittings used in the Agilent 1260 Infinity SFC Control Module use a nut and ferrule As the nut is tightened the ferrule compresses on the tubing creating a leak tight seal When correctly installed there is minimal additional volume All volume is well swept When improperly set the pilot does not fill the fitting leading to additional poorly swept volumes Figure 11 Compression fittings If over tightened the ferrule can compress the tubing and cause sufficient deformation to prevent removal of the fitting 42 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Installing Agilent 1260 Infinity SFC Control Module G4301A CAUTION Early connection may damage the instrument gt Do not connect AC power or interconnection cables or gas tubing to the Agilent 1260 Infinity SFC Control Module until these installation procedures direct you to do so Preparation Locate all modules devices and supporting equipment before continuing Ensure that the supply tubing can reach a physically secured source of CO Ensure t
39. detectors using the 10 mm flow cell This needs to be optimized empirically Standard ALS configuration two groove rotor Most Agilent automated liquid samplers ALS use the broken loop mode of injection with a 2 groove rotor One groove alternately connects the pump to either the column or to the back of the metering syringe The second groove alternately connects the needle port to either the waste port or to the column Loading position or Bypass position in CS In the first position pump to column needle port to waste the metering device in the automated liquid sampler is filled with the mobile phase at atmospheric pressure The back of the device inlet is dead headed against the rotor in the injection valve The metering device can then withdraw sample from a vial or air from the sample compartment to create segmented flow The sample is stored in the 1260 Infinity Analytical SFC System User Manual Introduction to Supercritical Fluid Chromatography SFC 1 needle and for large injections in the tubing in the arm upstream of the needle The rotor piston seal and all must be in good shape leak tight and properly maintained for accurate metering and aspiration of the sample To metering pump From pump Plug To column Towaste From needle port Figure 3 Loading position Injection position or MainPass position in CS The maximum injection volume with the standard metering device is 100 uL The piston is driven b
40. ect OFF in the Control window This shuts off the BPR heater and booster chiller and allows them to move toward ambient temperature This causes the BPR to home and fully open the CO path to depressurize The Agilent 1260 Infinity SFC Control Module unit contains approximately 25 mL of stored COs This amount of CO should be vented properly which takes several minutes You should allow the system to drain below 40 bar before cracking any fittings At this point the CO is in the vapor state and represents a small expanded volume However do not inhale vapor directly from a cracked fitting The concentration of CO emerging from a flow line even at low pressure can be dangerous or even lethal WARNING Avoid inhaling high concentration of CO gt Never inhale vapor issuing from an SFC flow line Exposure to concentrations of CO over 5 in air can be lethal Always keep tubes directed away your face CO is ubiquitous in the atmosphere but at high levels should be treated with the same care as other toxic chemicals Always wear gloves and eye protection for safety Avoid inhaling venting gas near open fittings Alternatively if the column oven contains a column switching valve one path may be jumpered without a column The reduced restriction will allow the system to depressurize much faster Further the isolated column can be exchanged immediately since the contained volume of COs is small 1260 Infinity Analytical SFC Syste
41. ection wash pump 4 The existing line blue capillary from the inlet of the Agilent 1260 Infinity SFC Autosampler metering device can be plumbed into the union on the wash pump transfer line 1260 Infinity Analytical SFC System User Manual 67 3 68 Installing the G4309A Agilent 1260 Infinity SFC System Positioning the waste line In normal operation the sample loop is switched from mainpass i n the high pressure flow stream to bypass out of the flow stream and connected to the seat capillary and waste As the valve switches the fluid in the loop expands and rushes out of the loop through the waste line If the waste line is positioned to empty into a liquid reservoir such as a WPA flush port the exiting fluid from the sample loop could splash the flush port fluid across the ALS The preferred positioning of the waste line is through the leak vent In this position the expanding fluid exits harmlessly into the leak tubing Alternatively a waste line can be fabricated that empties into the Agilent 1260 Infinity SFC Control Module gas liquid separator waste bottle Under no circumstances should the waste line be allowed to be unconstrained During operation of the injection wash pump this is the final exit of the wash fluid Installing the Agilent BCD Board The BCD Interface card Interface board BCD with external contacts and BCD outputs G1351 68701 and relay cable from the shipping kit are used to control the wash pu
42. egisters available by macros ation Abat O ROLD Method A Regiel Oteect Not gt RCFLD Status Name BoosterPres Type DOUBLE Numeric Value 100 805 Additionally it works with the ChemStation SendModule function Using this command you can send commands directly to the SFC module There are special commands allowing you to enable and disable diagnostic mode print SendModule SFC1 EnableDiag print SendModule SFC1 DisableDiag Enabling Diagnostic immediately shows additional status information in the Status window Additionally a separate configuration menu item shows up in Instrument gt More and Additional instrument curves are available in the Online plot Enabling Diagnostic mode requires a restart of Agilent ChemStation to show the Additional configuration item and Instrument curves 1260 Infinity Analytical SFC System User Manual 1260 Infinity Analytical SFC System User Manual 5 Using the Agilent 1260 Infinity SFC Control Module Powering up the Module 90 Power up Sequence and Operational Control States 91 Operational Control States 92 The OFF State 93 The STANDBY State 93 The ON State 94 Controlling the Agilent 1260 Infinity SFC Control Module through the Agilent ChemStation 95 Running a method on the SFC system 98 Shutting Down the SFC System 101 Partial Shutdown 101 This chapter provides information and hints on the use of the SFC System Apg Agilent Technologies 8
43. ents Weight Dimensions height x width x depth Line voltage Line frequency Power consumption Ambient operating temperature Ambient non operating temperature Humidity Operating altitude Non operating altitude Safety standards IEC CSA UL 11 2 kg 22 Ibs 140 x 345 x 435 mm 5 5 x 13 5 x 17 inches 100 240 VAC 10 Wide ranging capability 50 or 60 Hz 5 320 VA 150W 512 BTU Maximum 0 55 C 32 131 F 40 70 C 4 158 F lt 95 at 25 40 C 77 104 F Non condensing Up to 2000 m 6562 ft Up to 4600 m 15091 ft For storing the module Installation category II Pollution degree 2 For indoor use only Table 13 Performance Specifications Type Specification Column Column capacity Switching valve Temperature range Column compartement temperature accuracy Column compartement temperature stability Active solvent pre heating and post conditioning Automated method development Up to 300 mm length x 4 6 mm ID or less Up to 3 with additional 2 x TCCs up to 9 Optional 2 6 2 10 8 9 6 column selector Ambient 10 C to 100 C 0 5 C 0 05 C As standard Optional 1260 Infinity Analytical SFC System User Manual 37 2 Site Requirements and Specifications Specifications 38 1260 Infinity Analytical SFC System User Manual 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System
44. erties of the flow cell Use of Solvents Observe the following recommendations on the use of solvents Brown glass ware can avoid growth of algae Avoid the use of the following steel corrosive solvents Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like sulfuric acid and nitric acid especially at higher temperatures if your chromatography method allows replace by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2CHCly O gt 2COCl 2HCI This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol Chromatographic grade ethers which can contain peroxides for example THF dioxane di isopropylether such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides Solvents containing strong complexing agents e g EDTA Mixtures of carbon tetrachloride with 2 propanol or THF 1260 Infinity Analytical SFC System User Manual Appendix 9 Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com 1260 Infinity Analytical SFC System User Manual 141 Index Index A Ag
45. gaining popularity in method development and UV and MS based separation and purification A variety of parameters such as stationary phase selection mobile phase composition modifier type and concentration column temperature and system pressure can be easily manipulated to fulfill separation requirements by influencing optimizing and exploiting selectivity in SFC 1260 Infinity Analytical SFC System User Manual Introduction to Supercritical Fluid Chromatography SFC 1 Common flow path overview for packed column SFC instrumentation In commercially available SFC systems CO is initially pumped in liquid state and is brought into the supercritical state by heating it above the critical temperature before it enters the high pressure area of the LC instrument After high pressure mixing with a modifier the mobile phase passes through the injection loop where the sample is introduced into the supercritical stream and further transported to the separation column The high pressure of the mobile phase must be maintained downstream of the detector outlet using a backpressure regulator to keep the mobile phase in its supercritical condition over the complete flowpath 1260 Infinity Analytical SFC System User Manual 11 1 introduction to Supercritical Fluid Chromatography SFC The Agilent 1260 Infinity Analytical SFC System The Agilent 1260 Infinity Analytical SFC System G4309A consists of a binary HPLC SFC pump G4302A a degasser
46. ged fittings need only an additional 1 8th turn once finger tight In Supercritical Fluid Chromatography the fluid has 1 10th the viscosity of water so this may not be tight enough All connections should be checked for leaks and tightened further if necessary Soapy water or Snoop make it easy to find leaks if carbon dioxide is in the fluid Tiny bubbles appear in the liquid around the fitting Each fitting should be individually and carefully installed The depth of the tube inside the fitting is very important If the tube pilot length beyond the ferrule end is too long the fitting can leak or after excessive tightening bind permanently If the pilot is too short a poorly swept volume can be created This poorly swept volume will create noticeable chromatographic tailing If the pilot is much too short the fitting could fail under use Pilot depths are not always interchangeable between fittings It is a best practice to swage a tube in the fitting in which it will be used It is best to provide some light force to hold the tube in the fitting and prevent the tube from exiting while tightening the fitting Excessive force can result in breakage of some components and should obviously be avoided It may be more expedient to replace the whole fitting if one of the connections fails to seal You may notice that some of the more expensive components such as a pressure transducer have a less expensive fitting mounted to them to act as a sa
47. gilent 1260 Infinity SFC Autosampler Figure 38 Autosampler Valve p n Description 0101 1409 3 Groove rotor seal 0101 1248 Sample Loop 5pl NOTE For all other Part Numbers please refer to the G1329B User manual 122 1260 Infinity Analytical SFC System User Manual Parts for Maintenance 7 Agilent Module Parts DAD SFC Parts Figure 39 DAD Flowcell SFC p n Description G4301 60100 SFC Flow Cell 79883 68700 High Pressure Flow cell refurbishment Kit NOTE For all other Part Numbers please refer to the G1315 65C User manual 1260 Infinity Analytical SFC System User Manual 123 7 Parts for Maintenance Agilent Module Parts 124 1260 Infinity Analytical SFC System User Manual 1260 Infinity Analytical SFC System User Manual 8 Identifying Cables SFC Control Module Cables 126 Overview 127 BCD Cables 128 External Contact Cable 130 CAN LAN Cables 131 RS 232 Cables 132 This chapter provides information on cables used with the Agilent 1200 Infinity Series modules ott Agilent Technologies 125 8 Identifying Cables SFC Control Module Cables p n Description 00 84 2040 Relay Cable HD15M F VGA type 6 00 84 2020 BNC Cable 00 84 2030 Remote Cable DB9 M M 00 84 2090 USB Cable 6 126 1260 Infinity Analytical SFC System User Manual Identifying Cables 8 Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC reg
48. ground connection or the use of unspecified power cord can lead to electric shock or short circuit gt Never operate your instrumentation from a power outlet that has no ground connection gt Never use a power cord other than the Agilent Technologies power cord designed for your region Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury gt Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations 1260 Infinity Analytical SFC System User Manual 25 2 26 Site Requirements and Specifications Bench space Agilent 1260 Infinity SFC Control Module The Agilent 1260 Infinity SFC Control Module requires approximately 1 foot of linear bench space immediately adjacent to the target Agilent 1260 Infinity system stack Approximately 5 inches of free space is required behind the instrument for cable access and adequate air flow for ventilation Similar access to the rear of the 1260 Infinity system is also required to install cables and interface cards As mentioned earlier for optimal performance the rear air space should not be heated significantly above room temperature by the exhaust of other instrumentation in the lab rather hot exhaust should be vented or directed upward from the instrument The module is designed to be installed on either
49. h the upper tee slot on the side cover of the Agilent 1260 Infinity SFC Control Module The return transfer tube can then be fastened in the right port of the tee in the lower center of the BPR drawer Return transfer line Fa Figure 14 Connecting the SFC control module return Line 1260 Infinity Analytical SFC System User Manual 47 3 48 Installing the G4309A Agilent 1260 Infinity SFC System Hardware Installation Optimized Agilent 1290 Infinity Thermostatted column compartment Plumbing Supercritical Fluid Chromatography SFC is susceptible to increased noise due to poor thermal matching of components within the Agilent 1260 Infinity stack The refractive index of carbon dioxide is 50 times more susceptible to temperature changes than water Consequently thermal control in SFC is extremely important The Agilent 1290 Infinity Thermostatted Column Compartment TCC contains two thermal conditioning zones that can greatly increase system performance by matching temperatures of the mobile phase to the modules being used Each of these zones contains internal transfer lines that can be used to thermally condition the fluid flowing through them The two zones exist on the left and right side blocks within the TCC The block on the right side has a 6 uL internal conditioning volume that is used to precondition the mobile phase before it enters the column When using 150 mm or shorter columns place them
50. hat adequate venting is available and within reach of supplied waste systems This document describes a particular order of plumbing the system with plumbing and electrical connections described last These operations are performed at the rear of the systems Depending upon your individual installation you may wish to perform operations at the rear of the instruments first This is perfectly acceptable provided you can maintain access to supply connections to ensure integrity and leak tightness of fittings and connections 1260 Infinity Analytical SFC System User Manual 43 3 Installing the G4309A Agilent 1260 Infinity SFC System CAUTION Unpacking the Agilent 1260 Infinity SFC Control Module Damaged Packaging When you receive your Agilent 1260 Infinity SFC Control Module G4301A inspect the shipping boxes for any signs of damage If the shipping container or cushioning material is damaged notify the carrier and save the shipping material for inspection Save all materials until the contents have been checked for completeness and the instrument has been mechanically and electrically checked Signs of damage gt If there are signs of damage to the module please do not attempt to install or use the instrument 44 Delivery Checklist Compare the delivery checklist with the contents of the shipping boxes to ensure completeness of the shipment For parts identification see Parts for Maintenance on page 119 Please
51. he manual describes the following Introduction e Site Requirements and Specifications e Installing the System Configuring the System e Using the Agilent 1260 Infinity SFC Control Module e Maintenance and Repair Parts for Maintenance e Identifying Cables e Appendix Agilent Technologies 2010 2012 Printed in Germany 12 2012 G4301 90001 EE Agilent Technologies
52. horoughly checked for leaks Any leaks in the supply fittings can vent the CO supply 1260 Infinity Analytical SFC System User Manual 57 3 Installing the G4309A Agilent 1260 Infinity SFC System CAUTION Overtightening the fitting could damage the filter gt Use two wrenches when installing the CO supply line to the bulkhead filter entry connection on the back of the module Although the filter is captured and should not rotate there is a remote possibility that fittings inside the module could be loosened by severe stress on the nut on the supply line Leakage inside the cabinet requires service by trained personnel Gas Delivery Systems GDS Anyone performing semi prep SFC has probably been convinced that operation without a GDS is problematic Thus many laboratories are now plumbed with carbon dioxide boosted to 70 80 bar outlet pressure Even though an analytical system does not need such a GDS it is perfectly adapted to its use The Agilent 1260 Infinity SFC Control Module has an inlet safety shut off valve rated to 1500 psi gt 100 bar While this is rating is well above the outlet pressure of any typical GDS past experience suggests that it is wise to allow for some extra margin Agilent Technologies suggests setting the local output of any GDS between 60 bar and 70 bar through local outlet pressure regulators Under these conditions the GDS will almost always provide liquid carbon dioxide to the chromatogra
53. hrough the Agilent ChemStation 95 Running a method on the SFC system 98 Shutting Down the SFC System 101 1260 Infinity Analytical SFC System User Manual Contents Maintenance and Repair 105 Inspection and Preventative Maintenance Intervals 106 General Maintenance procedures 108 Parts for Maintenance 119 Agilent 1260 Infinity SFC Control Module Parts 120 Agilent Module Parts 121 Identifying Cables 125 SFC Control Module Cables 126 Overview 127 BCD Cables 128 External Contact Cable 130 CAN LAN Cables 131 RS 232 Cables 132 Appendix 133 General Safety Information 134 The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC 137 Radio Interference 138 Sound Emission 139 Solvent Information 140 Agilent Technologies on Internet 141 1260 Infinity Analytical SFC System User Manual 1260 Infinity Analytical SFC System User Manual 1 Introduction to Supercritical Fluid Chromatography SFC History of SFC 8 Theory of SFC 9 Benefits of SFC 10 Common flow path overview for packed column SFC instrumentation 11 The Agilent 1260 Infinity Analytical SFC System 12 The Agilent 1260 Infinity SFC Control Module G4301A 13 HPLC SFC binary pump G4302A 13 SFC Autosampler G4303A 14 The Column Compartment G1316C 21 UV detection DAD G1315C and MWD G1365C 21 Applications 21 Columns 22 This chapter provides an overview of the history theory and benefits of SFC ott Agilent Technologies 7 1 i
54. ical SFC System User Manual 63 3 Installing the G4309A Agilent 1260 Infinity SFC System Ball Valve OBV is installed with a Valve Holder on Pumphead B to allow the Channel B to be flushed even if CO tank pressure is supplied to the System On the Passive Inlet valve of the CO Channel Channel A is an Adapter to allow a Swagelok fitting to be connected to the valve The damper includes the pump pressure sensor and allows a pressure up to 600 bar Different set of piston seals are installed in the two pump heads Normal phase seals yellow PE in pump head channel A standard seals PTFE carbon filled in pump head channel AB WARNING Toxic flammable and hazardous solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks gt When working with these substances observe appropriate safety procedures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice gt The volume of substances should be reduced to the minimum required for the analysis gt Do not operate the instrument in an explosive atmosphere The BNC coaxial cable can be used to connect the Analog Output on the back panel of the Binary pump to the Agilent 1260 Infinity SFC Control Module Reference In terminal connector on the back of the SFC control module Be aware that the output
55. ifier flow at 5 mL min for 15 min followed by pure CO for 5 min 1260 Infinity Analytical SFC System User Manual 115 6 Maintenance and Repair Wash Pump Drain the inlet line of old solvent Flush the inlet line and filter from a small intermediate reservoir to rinse contaminated residual fluid from the lines 3 Insert the inlet line into a fresh supply of pure solvent 4 Prime the wash pump for 2 min four consecutive presses of the 30 s timer to clear the remaining flow path Plugged BPR Decontamination Decontamination of plugged BPR heads may require more aggressive solvents In this case use the following procedure ao a A whe Depressureize the SFC control module unit completely Disconnect the BPR inlet and outlet tubes from the BPR drawer Attach the Inlet tube via a transfer line to waste Attach a solvent pump to the outlet tube of the BPR head Prime the pump with a suitable solvent for the obstructing material Flush backwards with strong solvent at 1 mL min for 20 minutes Do not exceed a pressure of 400 bar If the pump cannot transfer fluid at less than 400 bar discontinue the operation and perform steps to exchange the BPR head If the backflush is successful rinse the BPR head with Isopropanol for 10 minutes at 1 mL min to clear the strong solvent Reconnect the BPR inlet and outlet lines 10 Complete the standard decontamination procedure listed above 116 1260 Infinity Analytical SFC System
56. ilent oninternet 141 algae 140 ambient non operating temperature 33 34 35 36 37 ambient operating temperature 35 46 37 BCD cable 128 127 c cable BCD 128 127 CAN 131 external contact 130 LAN 131 127 RS 232 132 127 cables overview 127 CAN cable 131 condensation 27 D dimensions 33 34 35 36 37 E electrostatic discharge ESD 69 external contact cable 130 142 33 34 F flow cell 140 solvent information 140 frequency range 33 34 35 36 37 H humidity 33 34 35 36 37 installation power cords 25 site requirements 24 internet 141 L laboratory bench 26 LAN cable 131 127 line frequency 33 34 35 36 37 line voltage 33 34 35 36 37 non operating altitude af non operating temperature 36 a7 0 operating Altitude 33 34 35 36 37 operating temperature 37 33 34 35 36 33 34 35 33 34 35 36 P physical specifications 37 power consideration 24 33 34 35 36 37 33 34 35 36 power consumption power cords 25 R RS 232C cable 132 RS 232 cable 127 S safety class 135 safety general information 135 standards 35 34 37 33 36 symbols 134 site requirements 24 solvents 140 specification physical 37 34 35 33 36 Specifications 28 V vacuum degasser 36 voltage range 33 34 35 36 37 Ww weight 33 34 35 36 37 1260 Infinity Analytical SFC System User Manual www agilent com In This Book T
57. is product is classed as a Monitoring and Control instrumentation product Do not dispose off in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com for more information 1260 Infinity Analytical SFC System User Manual 137 9 Appendix Radio Interference Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with equipment unscreened cables and or used for measurements on open set ups the user has to assure that under operating conditions the radio interference limits are still met within the premises 138 1260 Infinity Analytical SFC System User Manual Appendix 9 Sound Emission Manufacturer s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991 This product has a sound pressure emission at the operator position lt 70 dB e Sound Pressure Lp lt 70 dB A At Operator Position e Normal Operation e According to ISO 7779 1988 EN 27779 1991 Type Test 1260 Infinity Analytical SFC System User Manual 139 9 Appendix Solvent Information 140 Flow Cell To protect optimal functionality of your flow cell Avoid the use of alkaline solutions pH gt 9 5 which can attack quartz and thus impair the optical prop
58. iting the module may contain several percent organic solvent The effluent should NEVER be vented directly into an enclosed space occupied by humans because of the potential for long term exposure to toxic substances Locate and assemble the waste bottle and Tygon vent tubing The vent tubing can be placed over the spout on the top of the waste bottle Route the Tygon tubing to an appropriate vent The system must be actively vented Locate the SFC control module Waste line Insert the free end through a hole in the top of the waste bottle cap Insert the tube half way into the waste bottle Connect the fitting end to the outlet union on the BPR This union uses a 10 32 CPI fitting Tighten snugly Installing the Flowcell The back pressure regulator exists after any detectors in the HPLC system Thus the detector flow cells or splitter in the case on an ELSD or Mass Spectrometer operate at an elevated pressure relative to HPLC Agilent Technologies offers a Diode Array Detector DAD flow cell that has been extensively optimized for use in Supercritical Fluid Chromatography SFC This cell is pressure rated and tested to 400 bar It contains extensive 1260 Infinity Analytical SFC System User Manual 45 3 Installing the G4309A Agilent 1260 Infinity SFC System thermal conditioning not found in standard HPLC flow cells Agilent Technology s cell is highly recommended for SFC usage The flow cell should already be installed in the DA
59. ity SFC Control Module are the Nozzle Pressure system back pressure and the Nozzle Temperature temperature of the back pressure regulator 96 1260 Infinity Analytical SFC System User Manual Using the Agilent 1260 Infinity SFC Control Module 5 Controlling the Agilent 1260 Infinity SFC Control Module through the Agilent ChemStation Controlling the wash pump 6 6 O 0pt 00 500 a 3 000 mi min a 3748 C 39 99 190 400 nm Step 20nm WL BW RefWL RefBW mAU B 220 16 360 100 17 23 4 8 8 88 3 8 8 kal Change E aa w se ttt ey T kutrument 1 Uey When the wash pump icon is clicked the wash pump starts pumping for 30 seconds and flushes the autosampler metering loop needle and needle seat with solvent Typically modifier solvent is used to flush the autosampler The wash pump is controlled by the Agilent SFC autosampler via the built in BCD board and works independently of the current state of the Agilent 1260 Infinity SFC Control Module 1260 Infinity Analytical SFC System User Manual 97 5 Using the Agilent 1260 Infinity SFC Control Module Running a method on the SFC system Running a method on the SFC system Loading the SFC_Def analysis method When the SFC Driver add on for ChemStation is installed the method SFC_Def M is copied to the default method folder This method contains parameters most commonly used in SFC You should develop your SFC method
60. k Valve Holder A5 Wash Pump Check Valve PKG OF 2 Check Valve Gasket Inlet 5pk Check Valve Gasket Outlet C02 Supply Line Pump Transfer Line Return Transfer Line Wash Pump Transfer Line Wash Pump Transfer Line EVO Cross and Cap Kit for Aux Pres Sensor Pressure sensor Witness line short Pressure sensor Witness line long Manifold 6 to 1 for Column screening Thermal Isolation Cover Assy Booster Pump Piston Kit Heated Nozzle Assembly 1260 Infinity Analytical SFC System User Manual Agilent Module Parts Parts for Maintenance 7 Agilent Module Parts Agilent 1260 Infinity SFC Binary Pump TDA tea 5 g 0 oe Th y Q k gt 4 P O 3e 1 4 6 me ter Oe 8 ss hr sA 2 E S C amp 5 Figure 37 Agilent 1260 Infinity SFC Binary Pump specific SFC Parts p n Description G4302 20000 Adapter OV SFC 5023 1803 Adapter male female G1311 60065 G1312 87306 2x G1312 87300 G1312 60061 G1312 60067 G1312 60066 Damper 600bar with pressure Sensor Capillary 105x0 17 mm Absorber capillary Purge valve Outlet check valve Passive inlet valve G1312 04100 Mixer Clamp G1312 87330 Mixer 0905 1420 Pump seals PE PumpHead A 0905 1503 Pump seals PTFE PumpHead B 1260 Infinity Analytical SFC System User Manual 121 7 Parts for Maintenance Agilent Module Parts NOTE For all other Part Numbers please refer to the G1312B User manual A
61. ld Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms the warranty terms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcon tract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commercial item as defined in FAR 2 101 a or as Restricted computer soft ware as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or dis closure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly per
62. let and outlet lines Cleaning or Replacing Booster Pump Piston Tools for removing the vapor shield see Removing the vapor shield on page 109 and pump head see Removing the Pump head on page 111 A 9 64 hex drive wrench In most cases this procedure will be used only to replace a broken piston Pumping CO does not tend to leave deposits on the piston Development of such deposits warrants examination of the CO supply system and correcting the source of the deposited materials Release of extraneous materials into the CO supply system may cause contamination of the Agilent 1260 Infinity Analytical SFC System 1 Remove the Vapor Shield 2 Remove the pump head 3 Clean the pump head Take care not to break coolant tubes gt Use care removing the chiller assembly from the mounting posts The assembly is connected to a circulation pump behind the drawer panel Do not pull the flow lines hard as this may loosen or crimp the tubes and cause the chiller to lose efficiency or cause leaks in the secondary cooler system 1260 Infinity Analytical SFC System User Manual 113 114 Maintenance and Repair With a gentle rocking motion loosen the chiller plate assembly and carefully slide it forward off the pump head mounting posts Carefully twist the assembly out of the way Use the 9 64 hex wrench to unscrew the two cap screws attaching the spacer and very carefully remove the spacer by pulling straight back This
63. lling the G4309A Agilent 1260 Infinity SFC System The Agilent 1260 infinity stack requires a LAN connection to the PC This LAN connection requires all the normal HPLC ChemStation properties such as BOOTP Firewall and IP Address settings These remain unchanged in an Agilent 1260 Infinity SFC Control Module installation Connecting and operating multiple instruments on a single PC is not supported Both the Agilent 1260 Infinity SFC Control Module USB and Agilent 1260 Infinity LAN connections must be made on the PC on which ChemStation is installed and which is used for instrument control 60 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Hardware Installation Connecting the Leak Tray Waste Line The Agilent 1260 Infinity SFC Control Module contains a leak tray on the bottom of the instrument to collect and sense any liquid spills that may occur in the Agilent 1260 Infinity SFC Control Module cabinet In the bottom of this leak tray is an active sensor that continuously monitors for the presence of liquid The drip tray contains an overflow drain to divert any large amounts of collected liquid to an external collection container The overflow tube incorporates a simple push to connect fitting It is connected to the port on the bottom center on the front of the instrument Pushing on the outside ring of the port allows this line to be removed Since this liquid may be organic sol
64. losure Insert the filter closure into the housing and tighten 1260 Infinity Analytical SFC System User Manual Maintenance and Repair 6 Replacing Fuses The power entry module of the Agilent 1260 Infinity SFC Control Module unit contains an external fuse drawer that is user serviceable To replace fuses before replacing fuses first try to determine cause of fuse activation and repair 1 Power down the unit 2 Disconnect the power cable from the power entry module 3 Depress the release lever of the fuse drawer and pull the drawer straight back to remove 4 Replace blown fuses with 8 A250 V Time Delay fuses of matching size A set of replacement fuses is included shipping kit 5 Replace the fuse drawer by sliding it into the power entry module until it locks into place Standard Decontamination Cleaning External surfaces of the enclosure can be wiped with a damp soft cloth More stubborn marks can be removed with a 50 isopropanol water mixture or mild cleanser such as Soft Scrub The latter may also be used to remove surface paint blemishes that may result from normal use The vapor shield of the booster drawer should be wiped only with a very soft cloth such as a microfiber polypropylene cloth otherwise the surface may be scratched Other user accessible internal surfaces can be cleaned with a damp cloth BPR The BPR head contacts COs modifiers and sample material To decontaminate rinse with 50 mod
65. lvent See the plumbing scheme Figure 19 on page 53 There is an extra in line check valve downstream of the wash pump This check valve contains a ball pushed into a seat using a spring The purpose of the spring is to prevent siphoning of the wash solvent from the container through the injection valve to waste With the check valve in place it is easy to prime the injector wash pump without siphoning Once the wash pump transfer line and spring loaded check valve are connected to the injector wash pump you can fill the pump through the injector wash pump transfer line A syringe and several Luer adapters are included in the ship kit see Figure 20 on page 54 The syringe can be connected to the wash pump transfer line once the union is removed using the Luer adapter Retracting the syringe pulls solvent through the system check valves and tubing This effectively primes the injector wash pump After priming remove the Luer adapter reinstall the union and connect to the autosampler metering device 1260 Infinity Analytical SFC System User Manual 53 3 Installing the G4309A Agilent 1260 Infinity SFC System Syringe Wash pump transfer line D D gt d Luer fitting map Check valve temporarily removed Figure 20 Priming the wash line Connecting Agilent 1260 Infinity SFC Control Module to a Source of Carbon Dioxide The Agilent 1260 Infinity SFC Control Module has a 1 8th inch tube inlet connection on the lower left
66. m User Manual 103 5 Using the Agilent 1260 Infinity SFC Control Module System contains always 25 ml liquid CO2 under pressure gt The Agilent 1260 Infinity SFC Control Module unit contains approximately 25 mL of liquid CO The CO must be vented properly since the expanded volume will allow local concentrations exceeding the OSHA PEL Always allow the system to depressurize to below 40 bar before cracking any fittings Always keep fittings directed away from the face 104 1260 Infinity Analytical SFC System User Manual 1260 Infinity Analytical SFC System User Manual Maintenance and Repair Inspection and Preventative Maintenance Intervals 106 Daily Inspection and Maintenance 106 Every 3 months 107 As Needed Corrective 107 General Maintenance procedures 108 Booster Drawer 108 Replacing Fuses 115 Standard Decontamination 115 Plugged BPR Decontamination 116 Preparing for storage or shipping 117 In this chapter only the SFC specific procedures are described For procedures similar to the Agilent module procedures please refer to the single module manuals G1312C G1329B G1316C G1315 65C G4225A ae Agilent Technologies 105 Maintenance and Repair Inspection and Preventative Maintenance Intervals 106 Inspection and maintenance of the Agilent 1260 Infinity Analytical SFC System are critical elements of long term reliability and performance of the system Maintenance falls into two categories preventative and corrective
67. mp A IN b f Z A BCD Interface card Ad Ga 2 ANNA Figure 29 BCD Interface Card Agilent HPLC autosamplers have a small compartment located on the back panel near the top with a cover held in place by two captured knurled nuts 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Loosen the nuts and remove the cover taking care to retain it for future use Take the BCD Interface card from the shipping kit taking care to prevent damage from static electricity solvent etc CAUTION Electronic boards are sensitive to electrostatic discharge ESD and should be handled with care so as not to damage them Touching electronic boards and components can cause electrostatic discharge ESD can damage electronic boards and components gt Be sure to hold the board by the edges and do not touch the electrical components Always use an ESD protection for example an ESD wrist strap when handling electronic boards and components 1 Carefully slide the board into the slot When it is fully in place gently push the bezel until the connectors engage Tighten the captive knurled nuts 2 With the BCD card in place connect the 15 pin relay contacts connector to the relay input connector on the back of the SFC control module 3 Connect the 9 pin Remote connector on the back left of the autosampler to the 9 pin Remote connector on the back of the SFC control module
68. nstallation Complete 1260 Infinity Analytical SFC System User Manual 3 77 3 Installing the G4309A Agilent 1260 Infinity SFC System Software Installation 78 1260 Infinity Analytical SFC System User Manual 1260 Infinity Analytical SFC System User Manual 4 Configuring the System Configuring SFC interface in ChemStation 80 Setting up the Method 84 Status 86 Control 87 Testing the System 88 How to configure the Agilent 1260 Infinity SFC Analytical system and Agilent 1260 Infinity SFC Control Module in ChemStation aa Agilent Technologies 79 4 Configuring the System Configuring SFC interface in ChemStation Configuring SFC interface in ChemStation NOTE The Agilent 1260 Infinity SFC Control Module ChemStation interface works with the ChemStation Modular LC System not with Modular LC System Classic The Modular LC System Classic instrument does not support RC Net drivers which are necessary for the LC modules 1 Select Modular LC System as instrument type j Configuration Editor Histrument I Select Instrument eee J f Instrument Type ey LLC Data Analysis onl Instrument 1 Modular LC System Classic instrment 1 Modular LE System Instrument Name LC System Access Instrument 1 Access Point E Cc Initial Screen Window Size Nomal Icon Fullscreen Cancel Help 2 Start the Agilent ChemStation 3 Configure the devices in the Agilent ChemStation see Agilent ChemSta
69. nsure that the sample reaches the loop Withdraw Run r Waste Waste Needle J Needle 4 Load Column 4 Pump Column Pump Inject Rotate 4 Waste was A 2 5 2 5L Column Pump 4 5 rotate valve lt lt Column Pump Figure 31 Full Loop Injection 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Draw air bubble Draw 2nd air bubble o lt Needle Needle Needle Waste Waste Waste Column M trump Column t Pump Column 4 Pump Needle a Needle t Waste Column 4 4 Pump Column t Pump Figure 32 Partial Loop Injection Some General Injection Rules 20 uL loops are commonly used in HPLC In SFC the sample is often dissolved in a solvent that is stronger than the mobile phase Injecting large volumes such as 20 uL of such a solvent will cause peak distortion As a rule of thumb no more than approximately 5 uL of a polar solvent such as methanol should be injected onto a 4 6 mm ID column as shown in Figure 33 on page 74 This should NOT have a major impact on area reproducibility but should destroy efficiency as indicated in Figure 33 on page 74 1260 Infinity Analytical SFC System User Manual 73 3 Installing the G4309A Agilent 1260 Infinity SFC System Use Small Loops The loop should not be much larger than the maximum desired injection or lt 5 uL Bear in mind that the loop is washed with a strong solvent and is
70. nted in the power supply WARNING Hazard of electrical shock or damage of your instrumentation can result if the devices are connected to a line voltage higher than specified gt Connect your instrument to the specified line voltage only WARNING The module is partially energized when switched off as long as the power cord is plugged in Repair work at the module can lead to personal injuries e g electrical shock when the cover is opened and the module is connected to power gt Always unplug the power cable before opening the cover gt Do not connect the power cable to the instrument while the covers are removed 24 1260 Infinity Analytical SFC System User Manual CAUTION Site Requirements and Specifications 2 Inaccessible power plug In case of emergency it must be possible to disconnect the instrument from the power line at any time gt Make sure the power connector of the instrument can be easily reached and unplugged gt Provide sufficient space behind the power socket of the instrument to unplug the cable Power Cords Different power cords are offered as options with the module The female end of all power cords is identical It plugs into the power input socket at the rear of the module The male end of each power cord is different and designed to match the wall socket of a particular country or region Absence of ground connection or use of unspecified power cord The absence of
71. ntroduction to Supercritical Fluid Chromatography SFC History of SFC Supercritical fluid chromatography SFC was first introduced by Klesper et al in 1962 Klesper E Corwin A H Turner D A J Org Chem 1962 27 700 for the separation and analysis of a porphyrin mixture using open tubular SFC The first commercial instruments using packed columns were available from Hewlett Packard HP in 1982 Since then several vendors have developed and commercialized packed column SFC instrumentation for analytical as well as for preparative separation SFC is widely accepted for the separation of chiral compounds and increased user interest has been observed for a wide spectrum of small to medium sized molecules due to the analysis speed achieved and the low solvent consumption The latest introduction of analytical SFC instrumentation the Agilent 1260 Infinity SFC Control Module coupled to an Agilent 1260 Infinity Binary LC system optimized for SFC 8 1260 Infinity Analytical SFC System User Manual Introduction to Supercritical Fluid Chromatography SFC 1 Theory of SFC Pressure Critical Pressure Critical Point Solid Critical Temperature Temperature Figure 1 State of a solvent The superior separation properties achieved by SFC can be explained best by the thermodynamics of liquids and gases see the phase diagram in Figure 1 on page 9 Above a critical pressure liquids can no longer enter the gaseous state
72. of similar appearance on the DAD and VWD detectors should NOT be used 64 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Hardware Installation Rear of SFC Bin Pump A ple Figure 26 Connecting the Analog Reference Signal 0 Power off l Power on 1260 Infinity Analytical SFC System User Manual 65 3 Installing the G4309A Agilent 1260 Infinity SFC System Hardware Installation Modifications to the Agilent Autosampler Valve Body Isolation Seal Spring to Back Aurora 3 Groove Rotor Seal Stator Head 9 64 hex screws Figure 27 Exploded View of the Autosampler Injection Valve NOTE Replacing a rotor seal is well documented in Agilent manuals and service videos Please refer to these guides for further assistance 66 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Hardware Installation 1 The Autosampler should be plumbed in accordance with Figure 28 on page 67 Metering Device SSA from pump Check Valve J Contained Waste to column Figure 28 Autosampler Fluidic connections 2 Connect one end of the wash pump transfer line with the check valve to the outlet port of the injection wash pump 3 Before connecting the union end of the wash pump transfer line use a syringe and Luer Adapter to prime pull sample through the inj
73. on the top of the inlet check valve cartridge with the flat side of the gasket facing the cartridge Inlet CV only 8 Insert the CV holder into the pump head and tighten with a 9 16 wrench 9 Refasten the inlet or outlet capillary line holding the CV holder with a 9 16 wrench and tightening the fitting with the 1 4 wrench to seal 10 Replace the vapor shield 1260 Infinity Analytical SFC System User Manual Tools required Parts required CAUTION Maintenance and Repair 6 Removing the Pump head 1 A 1 4 open end wrench A 9 16 open end wrench A 3 16 hex drive wrench seal insertion removal tool Ultrasonic bath lsopropanol Deionized water p n Description G4301 60220 Boaster pump piston kit Piston seal Each time the booster pump head is removed the piston seal should be exchanged since the seal surface may be easily scratched or distorted during removal For this reason the procedures are bundled Cleaning the pump head is optional after visual inspection Sealing surfaces of the pump head are critical to successful operation Never use metal tools or paper toweling to wipe probe or contact these surfaces a A Q N Set the SFC control module mode to OFF Wait for the pump head to reach room temperature Power off the SFC control module Remove the vapor shield Using the 9 16 and 1 4 wrenches remove the inlet line from the inlet check valve holder and the outlet line from the outlet check
74. ons 2 Ifa Thermostatted Autosampler is installed an additional 25 cm 10 inches of space on either side for the circulation of air and approximately 8 cm 8 1 inches at the rear is required for electrical connections If a complete 1260 Infinity system is to be installed on the bench make sure that the bench is designed to carry the weight of all the modules For a system including the Thermostatted Autosampler it is recommended to position the modules in two stacks Environment CAUTION Condensation within the module Condensation will damage the system electronics gt Do not store ship or use your module under conditions where temperature fluctuations could cause condensation within the module gt If your module was shipped in cold weather leave it in its box and allow it to warm slowly to room temperature to avoid condensation Ventilation WARNING Waste tube has to be connected to hood or vent gt The effluent from a supercritical fluid chromatograph may contain vaporized toxic solvents Never vent into an enclosed occupied space Always vent into a fume hood or vent to the outside 1260 Infinity Analytical SFC System User Manual 27 2 Site Requirements and Specifications Specifications System Specifications Type Specifications Flow range 0 1 mL min to 5 mL min settable 1 mL min to 5 mL min recommended Maximum operating pressure 600 bar Upgrade possibility of exisiting Yes 1100
75. ph Unlike some earlier systems the Agilent 1260 Infinity SFC Control Module easily condenses any fluid that is present as a vapor and prevent pump cavitations Cable connections to the HPLC Personal injury gt Ensure that the AC power cord is NOT yet connected to the instrument 58 Cable connections to the Agilent 1260 Infinity SFC Control Module are dependent upon the installed configuration The primary decision to be made is whether or not an Agilent autosampler is present When an Agilent 1260 Infinity SFC Autosampler is present the Agilent 1260 Infinity SFC Control Module remote line and relay contacts lines are connected to the autosampler 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Hardware Installation The Binary pump analog output signal should be connected to the Agilent 1260 Infinity SFC Control Module Reference in terminal Reference signal Remote signa Relay signal _ Figure 22 Reference Remote and Relay Signal Connections 0 Power off l Power on Lastly a cable should be connected to the Agilent 1260 Infinity SFC Control Module USB port This can be run to any convenient compatible USB port on the PC CAN cabling between the Agilent 1260 Infinity modules is unchanged from the normal recommended means of interconnecting HPLC devices 1260 Infinity Analytical SFC System User Manual 59 3 Insta
76. pre and post conditioning of the mobile phase In contrast flow rate mobile phase composition detection column temperature and data analysis are controlled by the modules of the Agilent 1260 Infinity SFC system in combination with the ChemStation software This includes metering the carbon dioxide flow and mixing the modifier into the mobile phase by the HPLC SFC binary pump In detail the Agilent 1260 Infinity SFC Control Module uses vapor phase carbon dioxide redestills it to the liquid state and boosts its pressure to just under the column head pressure Since the COs gas is a very poor solvent most contaminants in the carbon dioxide are left in the source which allows for the use of inexpensive beverage grade COs unlike in any other commercially available instrument The SFC control module further recollects the effluent from the UV or other detector and controls the backpressure up to 400 bar over the complete system In addition the SFC control module delivers the wash solvent to flush the fixed sample loop of the SFC autosampler HPLC SFC binary pump G4302A The HPLC SFC binary pump is equipped with passive inlet valves and with special seals and pistons to allow for CO pumping in channel A while channel B adds organic modifier for either isocratic or gradient performance Pumphead B is also equipped with a purge valve to allow for quick changeover of the organic modifier 1260 Infinity Analytical SFC System User Manual 1
77. pressure drops are not excessive 0 12 mm or 0 005 inch tubing can be selectively used Use ferrules and tubing connections as recommended by the equipment manufacturer All four degasser channels will be available for solvent usage It is highly recommended that one channel be reserved for neat methanol no additives Reserving this channel will minimize the time needed for flushing the degasser as solvents are changed Failure to adequately flush the degasser when switching solvents will greatly impact sensitivity Agilent 1260 Infinity SFC Binary Pump It is highly recommended that you familiarize yourself with standard maintenance functions and terminology used in the binary pump This information is available in the Agilent Binary pump reference manual and user guide Damper with build in Pressure Sensor pressure limit 600 bar and Clip for mixer lt gt a ywy E Agat Tochociogiss 4200 Capilary PV Valve Hold a T alve Holder Co Valve holder for third OB ae ates IN od l yoO Capillary ome Ly il Adapter male female B i a a Coiled Capillary Figure 25 Diagram of the Agilent Binary Pump The G4303A SFC Pump is a binary high pressure mixing pump optimized for the usage in a SFC System The Purge Valve is mounted on the right side for purging the Modifier Channel Channel B only An additional third Outlet 1260 Infinity Analyt
78. s Option Contact 1 Contact 2 Contact 3 Contact 4 2 0s 5 0 times Injection Volume No No Action NEEDLE down CONTACT B CLOSED WAIT 0 10 min CONTACT B OPEN VALVE bypass DRAW 1 5 uL from air def speed DRAW def amount from sample def speed def offset DRAW 5 uL from air def speed NEEDLE wash as method EJECT max amount into seat def speed VALVE mainpass start pulse CONTACT B CLOSED WAIT 0 10 min CONTACT B OPEN Open Open Open Open Using the Agilent SFC Autosampler as a fixed loop to external loop autosampler has several minor consequences that need to be understood to achieve adequate performance 1260 Infinity Analytical SFC System User Manual 71 Installing the G4309A Agilent 1260 Infinity SFC System Dead Volume Partial Loop Injections Plumbed as a loop injector the Agilent 1260 Infinity SFC Autosampler has a dead volume between the high pressure needle seat and the groove on the rotor of the injection valve Two different diameter tubes are used to make this connection Thus the actual dead volume can have several different values depending on the ID of the tubing that is used This dead volume can be several micro liters or more When attempting to make low volume injections it may be possible that no sample enters the loop unless precautions are taken Use an air bubble on each side of the sample insert a plug of modifier or other solvent behind the sample or any other method to e
79. s from this default method SFC_DEF M contains an injector program for full loop injection Eject maximum volume to seat with default speed using default offset 98 1260 Infinity Analytical SFC System User Manual Adjusting the Using the Agilent 1260 Infinity SFC Control Module 5 Running a method on the SFC system method for use The Injector timetable includes an additional flush of the Autosampler for 0 1 min by the wash pump By default the injection volume is 15 uL which corresponds to an overfill of the sample loop by approximately three times lt Sampler injector Program of Column Comp 37 DAD Instrument Curves Default Pump setting is 80 CO 20 modifier Typical Flow rate in SFC is 3 mL min however when SFC_DI should EF M is loaded the flow rate is set to 0 mL min Solvent compressibility be always set to no compensation for the CO Channel and to the corresponding value for the modifier 1260 Infinity Analytical SFC S ystem User Manual 99 Using t nfinity SFC Contr Running a method on the SFC system L g o Minimum Stroke Channel A Channel B so f0 gt 130 10 bar No compensation No compensation Pressure Limits Maximum Flow Gradient Min
80. s usually leads to additional effort to screen different columns in order to achieve optimum separation On the other hand it provides a valuable tool for achieving different selectivities for a given analyte mixture A review of column developments for SFC was recently published by T Berger B Berger amp R E Majors in LCGC North America May 1 2010 Figure 9 Where SFC Fits In from non polar to highly charged 22 1260 Infinity Analytical SFC System User Manual a 1260 Infinity Analytical SFC System User Manual e Se ee 2 Site Requirements and Specifications J i Site Requirements 24 Power Considerations 24 Power Cords 25 Bench space 26 Environment 27 Ventilation 27 Specifications 28 System Specifications 28 Specifications 28 Agilent 1260 Infinity System 32 This chapter provides information on environmental requirements physical and performance specifications only for the G4309 Agilent 1260 Infinity Analytical SFC System Apg Agilent Technologies 23 2 Site Requirements and Specifications Site Requirements A suitable environment is important to ensure optimal performance of the instrument Power Considerations The module power supply has wide ranging capability It accepts any line voltage in the range described in Table 5 on page 33 Consequently there is no voltage selector in the rear of the module There are also no externally accessible fuses because automatic electronic fuses are impleme
81. safety related parameters Updates the event log V Pressure and temperature sensors are continuously powered and sensed Y Coolant and electronics bay fans are continuously powered V The wash pump is activated by contact closure of the external contacted board placed in the SFC Autosampler independent of the Agilent 1260 Infinity SFC Control Module control state 1260 Infinity Analytical SFC System User Manual Using the Agilent 1260 Infinity SFC Control Module 5 The OFF State The OFF state is characterized as follows V The COs supply valve is closed unpowered V The booster pump drive is unpowered V The BRP drive is unpowered V The BRP heater is unpowered V The chiller is unpowered V The secondary cooling circuit pump is unpowered The OFF state is always entered after a successful power up sequence It can also be entered by selecting the Off option in the control window by a timeout from the STANDBY state or by pressing Off in the Agilent ChemStation graphical user interface twice in succession When the Agilent 1260 Infinity Control Module is in the OFF state the top power status light is constant and the bottom ready status light is off The STANDBY State The STANDBY state is characterized as follows V The CO supply valve is closed unpowered V The booster pump drive is unpowered V The BRP drive is powered V The BRP heater is powered V The chiller is powered V The secondary cooling
82. side of the 1260 Infinity system stack with sufficient high pressure transfer tubing to attach to a double stacked system If the 1260 Infinity system is attached to a split flow detector such as Mass Spec or ELSD the Agilent 1260 Infinity SFC Control Module should be positioned on the opposite side of the stack Shelves overhanging the Agilent 1260 Infinity SFC Control Module should provide a minimum of 6 inches of clearance to allow access to the rear power switch Finally the PC system interface to the Agilent 1260 Infinity SFC Control Module is USB 2 0 A six foot cable is supplied with the system The CPU must be placed within range of this cable Alternately the user may supply an extended length USB cable not to exceed 16 feet While the Agilent 1260 Infinity SFC Control Module can exist on either side of the 1260 Infinity system it is often easier to locate it on the left side For more specification details see Agilent 1260 Infinity SFC Control Module on page 28 Agilent modules The dimensions and weight of your module see Agilent 1260 Infinity System on page 32 allow it to be placed on almost any laboratory bench It needs an additional 2 5 cm 1 0 inches of space on either side and approximately 8 cm 3 1 inches at the rear for the circulation of air and electric connections The module should be operated in a horizontal position 1260 Infinity Analytical SFC System User Manual Site Requirements and Specificati
83. side on the back of the module This connection is actually part of a very high surface area filter intended to intercept catastrophic levels of particulates You need to connect this input to a source of carbon dioxide The most common source of carbon dioxide is liquefied carbon dioxide from a room temperature cylinder At room temperature the pressure in the cylinder could change from a little above 50 bar to just below 70 bar Unlike most SFCs Agilent 1260 Infinity SFC Control Module is immune to the variations in flow resulting from cylinder pressure WARNING Creating severe frostbite in a short time gt Expanding carbon dioxide can become extremely cold capable of creating severe frostbite in a short time Avoid contact with expanding gases Do not vent substantial quantities into the laboratory WARNING Use the system in a well ventilated area gt Carbon dioxide is poisonous at high concentrations and should only be used in well ventilated areas The system effluent should be vented into a fume hood or to the outside Evacuate if a large spill occurs A carbon dioxide sensor alarm is recommended 54 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Individual cylinders WARNING CO cylinders can be dangerous if handled improperly gt Carbon dioxide in cylinders is partially liquefied under high pressure and contains a great deal of energy If containmen
84. st to waste Additionally if this dead volume loss is not accounted for 2 uL of sample will not be injected For 1260 Infinity Analytical SFC System User Manual 17 1 18 Introduction to Supercritical Fluid Chromatography SFC example the metering device delivering 5 uL of sample may only result in 3 uL of sample making it into the sample loop External loop in To From pump waste To column External From loop out needle port Figure 6 Injection position Partial loop injections For partial loop injections with the three groove rotor the metering device accuracy is more important Accuracy and reproduci bility are determined by the metering device not by the loop volume The most effective way to accomplish a partial loop injection is to e include two air gaps one before and one after the sample plug Full fixed loop injection also has these two air gaps to prevent sample loss as the needle moves out of the sample vial and into the needle port e use a careful choice of air volumes to position the sample plug in the middle of the loop The air gaps are extremely effective in controlling the shape and volume of the sample plug Small air bubbles do not affect the chromatography A detailed procedure on how to use the Agilent 1260 Infinity SFC system for reproducible partial loop injection is described in Technical Note Injecting variable volumes using the partial loop fill method with the Agilent 1260 Infinity analy
85. standards for the connection of carbon dioxide cylinders They do not appear to change at national borders some users in one country have different supply connections from other users in the same country Agilent Technologies recommends that customers in Europe contact their gas supply companies and ask them how to mate the cylinders they supply with an American 1 8 OD supply line This should require a cylinder connector and a reducing union down to a 1 8 inch compression fitting Leaks will not be sensed or protected gt Carefully check supply cylinders and inlet fittings for leaks Any leaks present in the supply line and inlet fitting will not be sensed or protected by safety features in the module 56 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC System 3 Hardware Installation a CGA 320 with Gasket R EN Nort America only 7 msze Country specific adappter not included fi fee CO Supply line Assembly g _ a 1 8 inch Swadgelock A Figure 21 Figure 3 25 0 Power off l Power on Improper plumbing can cause leaks gt Itis imperative to use two wrenches to install the supply fitting in the bulkhead filter entry connection on the back of the module Turning or twisting the bulkhead supply filter could cause failures or leaks in tubing within the module gt All supply fittings need to be t
86. surized and slowly bleeds pressure through the nozzle A residual pressure remains in the system when the nozzle closes fully at lower pressure The booster remains chilled and much of the startup CO is preserved You should be aware that the system is pressurized and not to attempt maintenance under these conditions The detector and column oven are left in the ON state to maintain their readiness You may elect to exit the ChemStation in this state and should answer NO to the Shutdown Lamps query that appears during shutdown Restarting the ChemStation brings the system to this same state If more than two hours elapse in STANDBY mode the Agilent 1260 Infinity SFC Control Module enters the OFF state and pressure may be lost at a more rapid rate 1260 Infinity Analytical SFC System User Manual Using the Agilent 1260 Infinity SFC Control Module 5 Depressurizing the system When maintenance is required on the SFC system such as replacing the column the system should be depressurized It is not necessary to shut down all modules but only the pumps and any other devices undergoing maintenance To depressurize the system stop the Agilent 1260 Infinity SFC Control Module and the binary pump In the Control menu of the Agilent 1260 Infinity SFC Control Module booster the standby state will be selected check the Depressurize box and click OK If the Agilent 1260 Infinity SFC Control Module unit itself is to be serviced sel
87. t cabinet on top of the Agilent stack gravity can generate an additional 1 2 psi of pres sure on the wash pump The outlet check valve on the wash pump has a 15 psi spring pushing the ball into the seat If this check valve is damaged there is potential for wash solvent siphoning through the wash pump then through the metering device arm needle and needle port displacing some of the sample from the loop and causing loss of precision A quick check for this condition is simply to put the wash solvent bottle on the bench below the wash pump This removes the pressure differential and the siphoning will stop 1260 Infinity Analytical SFC System User Manual 19 1 20 Introduction to Supercritical Fluid Chromatography SFC The Agilent 1260 Infinity Analytical SFC System Troubleshooting Conversion of the ALS two groove rotor to a three grove rotor for SFC can only negatively affect reproducibility and carryover under the following conditions 1 The user is NOT running the supplied injector program Injector Program INSTRUMENT 1 Function Amount Destination Speed pl min 1 EJECT MAX SEAT bd DEF Program Lable Command SCOn OK e wn BS 4 i L Figure 8 Injector program 2 The user is running a standard broken loop injection method 3 A two groove rotor is being used 4 The tube that connects the wash pump in the SFC control module to the inlet of the metering pump syringe in
88. t cover 1 Set the Control state to OFF on the SFC control module 2 Wait for the chiller temperature to approach room temperature to prevent significant condensation on the chiller assembly and pump head 3 Turn the power OFF on the SFC control module Unplug the power cord 4 Remove the front cover of the SFC control module unit by pulling gently at the upper left and right indents to the rear of the cover The cover will release from its magnetic catch Lift the cover upward to clear the two mounting pins at the base and set it aside The 3 16 hex wrench used to remove the vapor shield and pump head is stored inside the removable front cover 5 While holding the vapor shield with one hand use the 3 16 hex wrench to loosen the four cap screws attaching each corner of the shield until they each disengage from the front panel The screws are captured in the shield do not try to remove them completely 6 Remove the shield and store it in a safe location Do not use a container for disassembled parts This will scratch the plastic and impair visibility of the pump head during operation Replacing the vapor shield 1 Locate the vapor shield approximately over the mounting holes in the booster drawer front panel 2 Engage each screw approximately one turn 3 Inspect the border of the vapor shield to make sure it is in sealing contact with the foam seal of the drawer face Adjust as necessary 4 Tighten the mounting screws to ens
89. t is breached a break in the line or cylinder the entire contents will vaporize and quickly expand up to 500 times in volume and create very forceful high velocity gas streams Cylinders must be properly constrained and proper tubing used to avoid damage that could generate projectiles Any industrial grade of carbon dioxide is acceptable provided it is supplied in a cylinder without a DIP tube Drawing off the vapor phase leaves non volatile contaminants behind in the cylinder Using cylinders with a DIP tube subjects the chromatograph to contaminants soluble in the dense liquid layer Larger tanks are more convenient in that they require to be changed less frequently Cylinders can contain up to 35 kg of CO3 Generally 4 6 mm columns are run at 3 5 mL min which is approximately 2 5 4 g min of carbon dioxide This is equivalent to 150 250 g h 1 2 6 kg day Thus a 15 kg cylinder should last 2 2 to 11 days a 25 kg cylinder would last 4 to 19 days and a 35 kg cylinder could last 5 3 to 27 days all depending on use 3 5 mL min 8 24 h day For individual users particularly new users the use of cylinders is perfectly acceptable Larger groups should consider installing a gas delivery system and a bulk storage tank Locate the cylinder as close to the instrument as possible In the past the cylinders were stored at much higher temperature than the lab temperature which resulted in vaporization in the supply line coming in
90. the Agilent ALS is not leak tight allowing the metering device to aspirate air 5 The other end of the tube is not tight allowing the syringe to aspirate air The wash pump is not delivering To check turn on the wash pump for 30 s and see if liquid drips out of the waste line from the injection valve 7 The check valve on the outlet of the wash pump is leaking allowing solvent to siphon 1260 Infinity Analytical SFC System User Manual Introduction to Supercritical Fluid Chromatography SFC 1 The Column Compartment G1316C The temperature of the mobile phase prior to detection is a critical parameter for minimizing baseline noise recorded in the detector flow cell The heat exchanger on the right side of the column compartment is used to pre heat the mobile phase before it enters the column indirectly heating the column The heat exchanger on the left side is used to change the temperature of the mobile phase to achieve minimum noise This is of crucial importance since the refractive index of carbon dioxide responds up to 50 times stronger than water based mobile phases thus even small changes in temperature can significantly affect noise levels Temperature changes of mobile phase with the left side heat exchanger e g between 38 C and 49 C resulted in a variation in peak to peak noise of over an order of magnitude The recommended temperature setting on the left heat exchanger in order to achieve minimum noise is typicall
91. the injection valve as shown Port 1 is connected to the inlet of the right side column pre heater thermal conditioning block of the oven Port 6 is connected to the output flow from the binary pump 1260 Infinity Analytical SFC System User Manual 49 3 50 Installing the G4309A Agilent 1260 Infinity SFC System Hardware Installation Connecting the Booster to the Agilent 1260 Infinity system Locate the stainless steel booster transfer line Connect one end to the top port of the output tee on the center right side of the booster drawer Tighten finger tight with an additional 1 8th turn as needed 7 cf T or O MEE A Pump transfer line assembly eee Se Figure 17 Connecting the Booster outlet line This tube can be routed through the tee slots on the side of the Agilent 1260 Infinity SFC Control Module The tube is routed upward between the SFC control module and the Agilent 1260 Infinity stack to the bottom side of the binary pump The tube is then routed horizontally to the bottom center of the binary pump where it can enter the concave opening behind the cover The tube should then be routed to the left side of the pump beneath the Channel A deft side The end of the booster transfer tube can then be installed with the adapter in the passive inlet valve Any spare tubing can be located between the SFC control module and HPLC
92. tical SFC System Agilent Technical Overview 5591 0514EN on www agilent com chem sfc Carryover For partial loop injections with SFC the sample is exposed to the inside and the outside of the needle the needle port two grooves and the sample loop One groove and the sample loop are washed by the mobile phase The other 1260 Infinity Analytical SFC System User Manual Introduction to Supercritical Fluid Chromatography SFC 1 two grooves are washed by the wash pump The fittings in the injection system must be leak tight to prevent drawing air bubbles into the metering device Both the two groove HPLC and the three groove SFC rotor settings have six potential leak spots in common However the three groove setting has one additional leak spot If the sample sits in the loop for any extended period of time there is the potential for a leaky fitting causing siphoning The waste line may be filled with solvent and sample Potential leak spots Figure 7 Potential leak spots in the loop waste line and the low pressure side of the injection system If the waste bottle is positioned substantially below the injection valve gravity can generate a 1 2 psi 0 1 bar pressure differential between the metering device and the waste bottle causing the system to siphon if there is a leaky fitting on the low pressure side of the injection system metering device arm needle needle port loop If the wash solvent is stored in the solven
93. tion Jor LC and CE Systems Installation Manual Chapter Configuring the Instruments Configuring a Modular 3D LC System or Modular LC System 1260 Infinity Analytical SFC System User Manual Configuring the System 4 Configuring SFC interface in ChemStation 4 Depending on the current configuration Agilent ChemStation startup phase asks if the configuration shall be modified Instrument configuration Do you want to update the instrument configuration C Suppress this message 5 In the instrument Configuration editor Auto Configuration sets up the Agilent system as usual Instrument Configuration Configurable Hodes Selected Modules Agilent 1100 1200 Series LC a Agilent 1100 1200 Series LC Auto Configuration Sa ipana GG Per ne 632a neses Divs Of cancere 1616C LP00000011 mP gt a ae BiPump D vain 1617604 LPononen20 IroPump x FLD 61321A I000EPP 1000 aP ColuminComp 2 Ask for configuration change at ChemStation startup CAUTION Conflict with SFC macro implementation gt It is important that the SFC Control Module is listed below the Agilent pump otherwise the SFC will become pump 1 of the system which conflicts with the current SFC macro implementation The SFC macro always checks the first pump of the system for error or standby 1260 Infinity Analytical SFC System User Manual 81 4 Configuring the System Configuring SFC interface in ChemStation 6 To set
94. to the lab Most SFC pumps cannot condense this vapor and therefore cannot deliver CO Agilent 1260 Infinity SFC Control Module has a very powerful condenser designed to accept vapor phase COs Nevertheless it is always advisable to not stress any equipment Facilities and safety personnel often wish to store and mount the cylinders outside the lab sometimes quite far from the intended location of the instrument They should recognize that the transfer lines can hold large volumes equivalent to a large fraction of a cylinder particularly if tubing with large ID is used Shut off valves at both ends of a transfer line are not recommended unless one or both has a pressure relief valve or burst disk 1260 Infinity Analytical SFC System User Manual 55 3 Installing the G4309A Agilent 1260 Infinity SFC System Be sure the cylinder is properly constrained and cannot tip over Suitable chains or cylinder straps are required Cylinders in the USA and Canada use a CGA 320 cylinder adapter One is included in the module USA ship kit along with a 1 4 inch FNPT to 1 8 inch compression fitting and 6 feet of 1 8 inch OD stainless steel tubing The filter fitting sticking out the back of the Agilent 1260 Infinity SFC Control Module contains 1 8 inch nut and ferrule s which could be used with the supplied 6 feet tube or a longer user supplied tube to connect a cylinder to the SFC control module There are at least four different European
95. trument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or make any unauthorized modification to the instrument Capacitors inside the instrument may still be charged even though the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious personal injury are present in this instrument Use extreme caution when handling testing and adjusting When working with solvents observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used 1260 Infinity Analytical SFC System User Manual Appendix 9 The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC Abstract The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC adopted by EU Commission on 13 February 2003 is introducing producer responsibility on all Electric and Electronic appliances from 13 August 2005 z This product complies with the WEEE Directive 2002 96 EC marking requirements The affixed label indicates that you must not discard this electrical electronic product in domestic household waste Product Category With reference to the equipment types in the WEEE Directive Annex l th
96. tuals The Instrument Actuals have to be enabled 2 The available status information depends on the configuration e g Aux Pressure 3 The button in the upper left corner of the Status user interface allows you to either switch the device ON or put it into Standby mode O Standby Back Pressure 86 1260 Infinity Analytical SFC System User Manual m 4 Configuring the Syste Control The following steps show you how you can control your SFC instrument in the Agilent ChemStation 1 In Instrument gt More SFC you find more menu items that allow you to control the device directly 1 online Method and Run Control iigas Method Sequence View Abort Help Det Select Injection Source Set up Instrument Method zs More BinPump gt More 1290 Infinity TCC gt More Valve gt introl Easy Sequence More FLD gt l veresre Revisions amp Serial s Control Togggle On Off Reset Inj Wash 30 sec Instrument Configuration M Stal 2 To change the status of the SFC device and to Depressurize go to Instrument gt More SFC gt Control This displays the Aurora SFC Control dialog box Columns Aurora SFC Control Control On of Standby DePressurize 1260 Infinity Analytical SFC System User Manual 87 4 Configuring the System Testing the System 88 The SFC driver lists all available configuration method and status values in ChemStation r
97. ual 131 8 Identifying Cables RS 232 Cables p n Description G1530 60600 RS 232 cable 2 m RS232 61601 RS 232 cable 2 5 m Instrument to PC 9 to 9 pin female This cable has special pin out and is not compatible with connecting printers and plotters It s also called Null Modem Cable with full handshaking where the wiring is made between pins 1 1 2 3 3 2 4 6 5 5 6 4 7 8 8 7 9 9 5181 1561 RS 232 cable 8 m 132 1260 Infinity Analytical SFC System User Manual 1260 Infinity Analytical SFC System User Manual 9 Appendix General Safety Information 134 The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC 137 Radio Interference 138 Sound Emission 139 Solvent Information 140 Agilent Technologies on Internet 141 This chapter provides addition information on safety legal and web Ee Agilent Technologies 133 9 Appendix General Safety Information Safety Symbols Table 15 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect risk of harm to the operator and to protect the apparatus against damage Indicates dangerous voltages Indicates a protected ground terminal Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in this product The apparatus is marked with this symbol when hot surfaces are available A and the user sho
98. ulations Overview BCD cables p n G1351 81600 CAN cables p n 5181 1516 5181 1519 RS 232 cables p n G1530 60600 LAN cable p n 5023 0203 5023 0202 Description Agilent module to general purpose Description CAN cable Agilent module to module 0 5 m CAN cable Agilent module to module 1 m Description RS 232 cable 2 m Description Cross over network cable shielded 3 m for point to point connection Twisted pair network cable shielded 7 m for point to point connection 1260 Infinity Analytical SFC System User Manual 127 8 Identifying Cables BCD Cables One end of these cables provides a 15 pin BCD connector to be connected to the Agilent modules The other end depends on the instrument to be connected to Agilent Module to General Purpose p n G1351 81600 Wire Color Pin Agilent Signal Name BCD Digit module Green 1 BCD 5 20 Violet 2 BCD 7 80 Za Blue 3 BCD6 40 m Yellow 4 BCD 4 10 Black 5 BCD 0 1 Ras Orange 6 BCD 3 8 Red 7 BCD 2 4 Brown 8 BCD 1 2 Gray 9 Digital ground Gray Gray pink 10 BCD 11 800 Red blue 11 BCD 10 400 White green 12 BCD 9 200 Brown green 13 BCD 8 100 notconnected 14 notconnected 15 5V Low 128 1260 Infinity Analytical SFC System User Manual Identifying Cables 8 Agilent Module to 3396 Integrators p n 03396 60560 Pin 3396 Pin Agilent Signal Name BCD Digit module cE 1 1 BCD 5 20 2 2 BCD 7 80 Se 15
99. uld not touch it when heated up WARNING aia alerts you to situations that could cause physical injury or death gt Do not proceed beyond a warning until you have fully understood and met the indicated conditions CAUTION A CAUTION alerts you to situations that could cause loss of data or damage of equipment gt Do not proceed beyond a caution until you have fully understood and met the indicated conditions 134 1260 Infinity Analytical SFC System User Manual Appendix 9 General Safety Information The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements WARNING Ensure the proper usage of the equipment The protection provided by the equipment may be impaired gt The operator of this instrument is advised to use the equipment in a manner as specified in this manual Safety Standards This is a Safety Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards Operation Before applying power comply with the installation section Additionally the following m
100. up the SFC module scroll down the Configurable Modules slider until you see the SFC icon Select it with a double click or right arrow to move it to the Selected Modules panel Instrument Configuration Corfigurable Modde Selected Modules Fo Agilent 1100 1200 Series LC Auto E Vaha amp EnPurnp 61312A DE43616813 g CohennCompartemeriChsster aP Cokin Comgp 61316C LP00000011 PurovalveCuster Vave 611604 LP00000020 Q mnie Agilent 1120 CompactLC J Coros c 1642064 Ask fot configuration change at ChemStation startup 7 Select Configure to open the SFC configuration dialog box Instrument Configuration Configurable Moduler Selected Modules wee A Agilent 1100 1200 Series LC Auo Evae 6 BiePunp 119124 IDE 43516819 Of corrrecongrtenert ave of aunetene exec qPeo000aN e Pume aveusar prow IG 11604 LP00000020 AN sr FLD 61321A 000 PP1000 Agilent 1120 Compacil C AN sec H Comoacil C G4296A Ask tor configuissan change at ChamStabon startup There we unconfigured Modules 82 1260 Infinity Analytical SFC System User Manual Configuring the System 4 Configuring SFC interface in ChemStation 8 In the Aurora SFC Configuration enter the device name or use the default to identify the module within Agilent ChemStation Select a COM Port in the Aurora COM Port field Aurora SFC Configuration Instrument 1 Device Name Aurora COM Port
101. ure at least 50 compression of the foam seal by the shield 5 Replace the front cover by aligning the two base mounting pins and tilting forward to engage the magnetic catches 1260 Infinity Analytical SFC System User Manual 109 6 Maintenance and Repair Tools required Parts required CAUTION Replacing Booster Pump check valves A 1 4 open end wrench A 9 16 open end wrench p n Description 1 G4301 00200 Plastic cover with screws 1 Remove the vapor shield 2 Using the 1 4 and 9 16 wrenches loosen and remover the inlet or outlet capillary tube 3 Using the 9 16 wrench loosen and remove the desired check valve holder The check valve may or may not be extracted with the holder 4 The inlet check valve assembly includes a PEEK gasket Set this gasket aside for reuse Inlet CV only 5 Remove the defective check valve cartridge Do not mix up check valve directions gt The orientation of the CV cartridge is critical An arrow on the side of the cartridge indicates the direction of flow Make sure the cartridge is installed to allow flow in the proper direction when installed into the pump head 110 6 Insert the new check valve cartridge into the holder oriented correctly for the direction of flow arrow up The inlet check valve is inserted with the non filter end of the cartridge showing The outlet check valve is inserted with the filter end of the cartridge showing 7 Replace the PEEK gasket
102. ust be observed Do not remove instrument covers when operating Before the instrument is switched on all protective earth terminals extension cords auto transformers and devices connected to it must be connected to a protective earth via a ground socket Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury Whenever it is likely that the protection has been impaired the instrument must be made inoperative and be secured against any intended operation Make sure that only fuses with the required rated current and of the specified type normal blow time delay and so on are used for replacement The use of repaired fuses and the short circuiting of fuse holders must be avoided 1260 Infinity Analytical SFC System User Manual 135 136 Appendix Some adjustments described in the manual are made with power supplied to the instrument and protective covers removed Energy available at many points may if contacted result in personal injury Any adjustment maintenance and repair of the opened instrument under voltage should be avoided whenever possible When inevitable this has to be carried out by a skilled person who is aware of the hazard involved Do not attempt internal service or adjustment unless another person capable of rendering first aid and resuscitation is present Do not replace components with power cable connected Do not operate the ins
103. vailable for suitable exposure level lt 5000 ppm CO2 1260 Infinity Analytical SFC System User Manual Maintenance and Repair 6 Every 3 months Y Run nozzle diagnostic test V Run system leak test V Evaluate system calibration V Check chiller efficiency curve V If CO cylinders are used as supply change the cylinder seal approximately every 10 cylinders at the next tank change V Remove visible dust accumulation in the area of the module As Needed Corrective V Change booster and CO pump check valves V Change high pressure transfer lines with metal ferrules or PEEK end fittings after 10 20 reseals or when leaking V Change Booster piston rare V Exchange BPR head rare 1260 Infinity Analytical SFC System User Manual 107 6 Maintenance and Repair General Maintenance procedures General Maintenance procedures Booster Drawer Check valve cartrige Outlet CV holder Piston Chiller plate and spacer N Piston Retaining nut Check valve cartridge 7 Inlet CV holder Figure 36 Exploded view of Booster Components 108 1260 Infinity Analytical SFC System User Manual Maintenance and Repair 6 Removing the vapor shield The vapor shield is not shown in the graphic Figure 36 on page 108 Most maintenance procedures require removal of the vapor shield to access the underlying pump unit Tools required A3 16 hex drive wrench mounted on the back of the fron
104. vents you should supply an appropriate collection container F Leak tray waste line 7 16 Tygon 5 16 ID ae ban Figure 23 Leak Tray Waste Line 1260 Infinity Analytical SFC System User Manual 61 3 Installing the G4309A Agilent 1260 Infinity SFC System Preparing the HPLC Preferred Stack Arrangement To minimize delays and broadening caused by excessive tube lengths we recommend the following stack layout The Agilent 1260 Infinity SFC Control Module needs to be immediately adjacent to the LC stack but can be placed on either side In the preferred arrangement the degasser and solvent tray are located on the top of the stack These feed into the binary pump and the SFC control module injection wash pump The binary pump is located below the degasser and directly above the autosampler The thermostatted column compartment is located below the autosampler with the detector at the bottom of the stack p p Degasser Binary SFC Pump O SFC Autosampler 1 Thermostatted column compartment DAD or MWD tr Figure 24 Preferred order of Agilent HPLC Components 62 1260 Infinity Analytical SFC System User Manual Installing the G4309A Agilent 1260 Infinity SFC ae ih 3 ardware Installation It is recommended to plumb the system with small diameter tubing For general use 0 17 mm or 0 007 inch tubing should be used In more demanding applications where
105. y a stepper motor Full travel on the piston is accomplished using thou sands of motor steps Each step results in a displacement of 0 01 uL and reproducibility could approach or be better than 0 1 If all injector components are leak tight the accuracy of the metering device is the only component that should affect the reproducibility of injections A leaky needle port a worn rotor or stator in the valve or a worn piston seal in the metering device are the most likely causes of poor precision other than leaking fittings To metering pump From pump PI g To column To waste From needle port Figure 4 Injection position 1260 Infinity Analytical SFC System User Manual 15 1 16 Introduction to Supercritical Fluid Chromatography SFC Carryover Carryover is largely a function of the cleanliness of the outside of the needle or of a gap between the rotor and stator caused by wear In some models needle wash is provided to wash the outside of the needle between injections When the injection valve is switched to position two pump to metering device needle port to column Inject or MainPass the mobile phase passes through the metering device down the tubing through the needle and port and into the column The mobile phase pushes the sample out of the needle tube and washes these devices out There is no wasted sample All of the sample withdrawn from the sample vial is injected The valve is in this position most
106. y between 37 C and 40 C for G1315C or G1365C detectors UV detection DAD G1315C and MWD G1365C The system can be equipped either with a DAD G1315C or an MWD G1365C using a high pressure detector flow cell suitable for SFC 10 mm path length 13 uL volume with short transfer tubing to minimize peak broadening Electronic temperature control provides highest baseline stability and stable sensitivity values under fluctuating temperature and humidity conditions This feature aids greatly in minimizing detector noise and now enables impurity and EE enantiomeric excess analysis by SFC particularly when using elevated temperatures Applications SFC has gained a wide interest and acceptance in many small molecule applications because of its high separation speed and efficiency selectivity low operating costs and due to low generation of organic solvent waste Important applications have been developed for the analysis of pharmaceutical drugs natural products fatty acids vitamins pesticides lipids and chiral compounds See Figure 9 on page 22 1260 Infinity Analytical SFC System User Manual 21 1 introduction to Supercritical Fluid Chromatography SFC The Agilent 1260 Infinity Analytical SFC System Columns In contrast to reversed phase separation there is no universal stationary phase available for SFC separations Most typically used stationary phases are ethyl pyridine diol cyano amino Silica and SCX columns Thi
Download Pdf Manuals
Related Search
Related Contents
ESTACION METEOROLOGICA INALAMBRICA DE Origin Storage 250GB TLC SATA 2.5" StarTech.com USB2DVI Seagate 5400.3 Computer Drive User Manual Fiche Technique (FT) - Zep Industries :: Onderhoudsproducten Minka Lavery 6811-66 Instructions / Assembly GUIDE de la Ville - Ville de Noisy-le IDX Damper - Agilent Technologies QuickScan™ QBT21X1 - Streckkod System AB Graco 3A0732J User's Manual Copyright © All rights reserved.