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CombiFlash® Rf

+

User Manual

2-20

solvents. For proper operation of this function, Solvent 1 must
be the weak normal phase solvent (typically an alkane such as
hexane). Solvent 2 must be the strong solvent (such as ethyl
acetate). Solvent 3 is the weak reverse phase solvent (usually
water) and solvent 4 is the strong reverse phase solvent (such
as methanol or acetonitrile).

2.13.3 General Settings

Combi

Flash

Rf Name

(optional) – Use this option to name

your system. The name will appear in operational displays
and run summaries. This feature is useful when your
laboratory has more than one Combi

Flash

Rf system.

Time Zone

– Select your time zone from the drop-down list

box.

2.13.4 Set Date/Time

Click this button to open a window from which you can set the
system date and time.

To prevent unauthorized time changes, this feature is
password protected. The system is shipped with the password
set to

combiflash

. Use the Tools>Set Password menu

command to change this password for greater security.

2.13.5 Vapor Limit

The system has an internal vapor sensor that detects vapors
present in the immediate atmosphere. When the limit is
exceeded, the Combi

Flash

Rf will shut down to avoid a

hazardous condition.

Teledyne Isco recommends using the default setting of 25.
This value represents an organic vapor level slightly above the
ambient vapor level of a well-ventilated laboratory.

A setting below 25 could cause random alarms without
significant vapors present. If PeakTrak displays a Vapor Limit
alarm while the Vapor Limit is set at 25, perform the following
checks on your laboratory and the instrument:

• Ensure that no open containers or spills of organic

solvent are in close proximity to the system.

• Ensure that the system is located in a well-ventilated

area.

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Summary of Contents for CombiFlash EZ Prep

Page 1: ...sh Rf User Manual For indoor use only COPYRIGHT 2013 by Teledyne Isco 4700 Superior St Lincoln Nebraska U S A 68504 Phone 402 464 0231 Toll Free 800 228 4373 FAX 402 465 3022 Revision C May 2015 Part 69 5233 650 ...

Page 2: ...CombiFlash Rf User Manual ii ...

Page 3: ...Z Prep Systems 2 1 Unpacking the Unit 2 1 2 2 Instrument Location 2 3 2 3 Connect Power 2 3 2 4 Connect Solvent Lines Excludes EZ Prep 2 4 2 5 Connect Waste Lines Excludes EZ Prep 2 6 2 6 EZ Prep Plumbing Connections 2 9 2 7 External Gas 2 10 2 7 1 CombiFlash Rf Rf Lumen and EZ Prep 2 10 2 7 2 CombiFlash Rf Lumen or EZ Prep with ELSD only 2 11 2 8 Connect and Route Drain Lines 2 11 2 9 Position th...

Page 4: ...Install Collection Tube Racks 3 10 3 9 Turn on Power 3 12 3 10 Configure the System 3 12 3 10 1 Solvents 3 13 3 10 2 General Settings 3 13 3 10 3 Set Date Time 3 13 3 10 4 Vapor Limit Optional 3 13 3 10 5 Set Default Tube Volumes 3 14 3 10 6 User Preferences 3 14 3 10 7 Restart the system 3 17 3 11 Prime the Solvent Lines 3 18 3 12 System Verification 3 18 3 13 Installation Qualification Checklist...

Page 5: ...Z Prep Operation 5 16 5 5 1 Column Mounting 5 16 5 5 2 Sample Preparation 5 17 5 5 3 Starting the Separation 5 18 6 User Help Reference 6 1 1 PeakTrak Window Elements 6 1 6 1 2 Method File 6 2 6 1 3 Run File 6 3 6 1 4 How to get PeakTrak help 6 3 6 2 1 File 6 3 6 2 2 Method Editor 6 7 6 2 3 MS 6 7 6 2 4 Tools 6 8 6 2 5 Help 6 10 6 3 1 Main Window 6 11 6 3 2 Method Editor 6 17 6 3 3 Gradient Optimi...

Page 6: ...ion 7 3 7 1 4 Apple Mobile Digital Devices 7 4 7 1 5 Install and Configure the PeakTrak App 7 4 7 2 Direct Connection 7 4 7 2 1 Windows 7 Settings 7 5 7 2 2 Windows Vista Settings 7 7 7 2 3 Windows XP Settings 7 9 7 2 4 Windows 2000 Settings 7 11 7 2 5 Completing the Direct Connection 7 13 7 3 Direct Printing 7 13 8 Maintenance 8 1 System Standby and Shut Down 8 1 8 2 Preventive Maintenance 8 2 8 ...

Page 7: ...n L 8 15 8 6 8 Cleaning the Ionization Source Capillary 8 15 8 6 9 Replacement of Ion Source Housing 8 16 8 6 10 Overpressure Error 8 16 8 6 11 Check Valve Cleaning 8 17 8 6 12 Replacing Check Valves 8 18 8 7 Injection Valve Maintenance 8 19 8 8 Electrical Troubleshooting 8 19 ...

Page 8: ...CombiFlash Rf User Manual viii ...

Page 9: ...platform This installation guide will refer to the specific model name when the discussion is limited to a particular model or configuration 1 2 Product Overview The Teledyne Isco CombiFlash Rf flash chromatography system gives you high productivity automation programmable gradients UV detection and peak separation and automatic detection of columns and collection tube racks with the exception of ...

Page 10: ... a 10 100 mL min 150 psi system that pumps two solvents to form a binary gradi ent This configuration has an easily accessible fluid path that supports liquid or solid sample introduction and a fixed wavelength UV detector 254 nm Optionally the sys tem can be configured for full spectrum 200 400 nm UV detection with secondary monitoring manual solvent selec tion valves to form a binary gradient fr...

Page 11: ... psi system that forms a binary gradient by automatically selecting two solvents from four inlets This configuration has an automatic self cleaning injection valve for sample introduction and full spectrum UV 200 400 nm or UV vis 200 800 nm detection with secondary wavelength monitoring An internal air pump is used for post run col umn air purging active solvent level sensing and waste full bottle...

Page 12: ...f Lumen This system has the same high performance features as the Rf system but includes an internal evaporative light scattering detector ELSD Dur ing operation this detector can be combined with the UV 200 400 nm or UV vis 200 800 nm detection to isolate visible and UV absorbing compounds as well as compounds with little or no chromophores ...

Page 13: ...es a mass spectrometer with a detection range of 50 to 1200 Daltons Da PurIon PurIon S or 50 2000 Da PurIon L systems During purification this system can be combined with the UV 200 400 nm or UV vis 200 800 nm detector to isolate visible and UV absorbing compounds as well as compounds with specific molecular weights or mass ranges ...

Page 14: ...e capability to perform Preparative HPLC separations on the same sys tem used for flash chromatography It is available with all the detector combinations of the Rf including UV UV Vis Evaporative Light Scattering and the PurIon mass spec trometer In addition the system is capable of preparative HPLC separations at flow rates of up to 200 ml min and 3500 psi 241 bar ...

Page 15: ...r channels are independent including separate waste containers with full bottle detection All CombiFlash Rf systems are optimized for use with Teledyne Isco s RediSep Rf columns which are pre packed with a variety of media For example the CombiFlash Rf can purify samples from 4 milligrams to more than 33 grams using RediSep Rf columns loaded with 4 to 330 grams of silica gel Applications include p...

Page 16: ...hone and iPad Note Teledyne Isco recommends that you obtain assistance from your Information Technology department before attempting direct or network connections 1 3 1 Multiple Control Possibilities The system can be accessed from the built in touch panel and up to ten network devices The touch panel shares control with all connected devices The system performs the most recent command from any co...

Page 17: ...e solvent Humidity when connected to power 95 relative humidity maximum at 20 to 40 C Flow Rate Range 10 to 100 mL min 1 to 200 mL min Flow Rate Accuracy tested with water at 138 kPa or 20 psi 10 5 5 200 mL min Pressure Limit 2 1 034 kPa 150 psi Up to 1379 kPa 200 psi column dependent Pressure Accuracy 10 of full scale 5 of full scale Gradient Formation Binary gradient from 1 and 2 solvent inlets ...

Page 18: ... 800 nm UV Vis Wavelength Accuracy 5 nm Fraction Accuracy 2mL flow rate 60 Electrical Safety per EN 61010 1 Pollution Degree 2 Installation Category II Maximum Altitude 2000 meters Note 1 All specifications are subject to change Note 2 For Rf columns undetected by RFID the max pressure is limited to 50 psi Table 1 1 CombiFlash Rf 150 and Rf System Specifications 1 Continued ...

Page 19: ...n Pressure Limit 2 1379 kPa 200 psi Pressure Accuracy 5 of full scale Gradient Formation Binary gradient from solvent inlets 1 4 Solvent selection can be automatically controlled by the method Peak Detection Modes Slope or threshold Flow Cell Path Length 0 1 mm 25 UV Detection and Monitor Wavelength Selectable from 200 to 400 nm range Optional 200 to 800 nm UV Vis detector Wavelength Accuracy 5 nm...

Page 20: ...te 60 Electrical Safety per EN 61010 1 Pollution Degree 2 Installation Category II Maximum Altitude 2000 meters Note 1 All specifications are subject to change Note 2 For columns undetected by RFID the max pressure is limited to 50 psi Table 1 2 CombiFlash Rf Lumen Specifications 1 Continued ...

Page 21: ...lectrospray Ionization ESI or optional Atmospheric Pressure Chemical Ionization APCI Positive or Negative Ionization Mode SIM Sensitivity 10 pg Reserpine 100 1 S N RMS with SIM of m z Number of Solvents Binary gradient with any two of four solvents A third solvent can be used to add modifier at a fixed percentage Programmable Gradients Linear step isocratic Sample Injection Direct User Interface 1...

Page 22: ... to 40 C Flow Rate Range 1 to 200 mL min Flow Rate Accuracy 5 5 200 mL min Pressure Limit 2 1379 kPa 200 psi Pressure Accuracy 5 of full scale Gradient Formation Binary gradient from A1 A2 and B1 B2 solvent inlets Solvent selection can be automatically controlled by the method Peak Detection Modes Slope or threshold Flow Cell Path Length 0 1 mm 25 UV Detection and Monitor Wavelength Selectable fro...

Page 23: ... range from 100 to 240 VAC 50 60 Hz 300VA maximum typical Line cord is the disconnect device Line Frequency 50 60 Hz Ambient T emperature 20 to 40 C maximum temperature must be at least 15 C below the boiling point of the solvent Humidity when connected to power 0 to 95 non condensing Flow Rate Range 5 to 200 mL min Flow Rate Accuracy 5 5 200 mL min Pressure Limitb 241 bar 3500 psi Pressure Accura...

Page 24: ...as Consumption 2 5 SLPM Drift T ube T emperature Setting range 30 to 90 C Split Flow Rate 0 75 mL min 10 Spray Chamber Setting range 10 to 60 C Temperature limited to minimum of 5 C below ambient Electrical Safety per EN 61010 1 Pollution Degree 2 Installation Category II Maximum Altitude 2000 meters a All specifications are subject to change b For flash columns undetected by RFID the max pressure...

Page 25: ...olymer Carbon impregnated fluoropolymer tubing and 316 stainless steel tubing Drain Tubing Vinyl with FEP liner Process Valves PEEK PTFE perfluorelastomer PPS Sample Loading Cap 316 stainless steel Sample Loading Cap Seal PTFE Elgiloy a Injection Valve PTFE PCTFE PPS for prep valve Flowcell 303 SST Type ES Quartz SIMRIZ SZ485 Pump 316 stainless steel PTFE Elgiloy a Elgiloy is a registered trademar...

Page 26: ...ve A Flash drive may be inserted into this port for transferring files importing and exporting methods and performing system software updates 3 Adjustable Flash Column Mount The injection valve assembly and upper column mount slide along this mount so the system can accept a variety of column sizes 4 On Standby Switch 1 On 0 standby 5 Fraction Collector Arm and Drop Former The arm and drop former ...

Page 27: ...biFlash Rf according to its current mode of operation Modes include column equilibration sample injection elution column flushing valve cleaning and system purging The injection valve is not available on the standard Rf 150 systems 9 Upper Flash Column Mount Secures the column inlet 10 Lower Flash Column Mount Secures the column outlet 11 Top Shelf Allows storage of accessories and solvent bottles...

Page 28: ...through this tube to a user supplied container 14 External Detector All systems except the Rf 150 and Rf Lumen The system can accept an analog peak voltage signal from an external detector The system will process this analog signal to determine the presence of a peak using PeakTrak s slope or threshold algorithms See section 2 11 more information 20 21 17 13 15 16 22 18 14 19 23 ...

Page 29: ...re information on Rf 150 solvent inlet ports 20 Optional External Gas Port An inlet for an internal pump which supplies pressurized air or user supplied gas for solvent level sensing waste container full detection and system column purges The external gas should be regulated to 2 5 psig before connecting the source to this port The port is not present on the Rf 150 systems 21 Mains Power Connects ...

Page 30: ...6 Nitrogen Inlet Rf Lumen only Connects to the carrier gas supply 60 to 70 psig 27 External Detector Rf Lumen only Reserved for future use 28 P trap Drain Rf Lumen only During operation condensate from the Thermo split process drains from the system An internal P trap prevents aerosol particles from escaping through this drain 29 Pump Drain Rf Lumen only An internal drip tray is located below the ...

Page 31: ...ir or user supplied gas to measure the hydrostatic pressure of the waste above the level sense line end The system will suspend operation when this level is too high Four ports allow you monitor the level of each waste container on the Rf 4x system 31 Column Waste Waste fluids are sent out ports 1 through 4 Tubing connected to these ports are paired with the waste level sense air lines and routed ...

Page 32: ...outine to this shared port 34 A B Reserved for future use 35 USB Cable This cable connects to the USB port on the Rf system back panel see item 16 The Rf system controls the operation of the Rf 4x module through this connection 36 Mains Power Connects the module to AC line voltage 37 Waste Level Sense From Rf Receives pressurized air or optional external gas from the Rf system ...

Page 33: ...d local regulatory laws and in compliance with your company s chemical hygiene plan in the event of a spill WARNING If you are using flammable solvents or chemicals with this system vapor concentration levels may exceed the maximum exposure levels as recommended by OSHA Guide 1910 1000 To reduce those levels to a safe exposure Teledyne Isco recommends that you place the system in a laboratory hood...

Page 34: ...tial hazard which if not avoided may result in minor or moderate injury This category can also warn you of unsafe practices or conditions that may cause property damage WARNING Warnings identify a potentially hazardous condition which if not avoided could result in death or serious injury DANGER DANGER limited to the most extreme situations to identify an imminent hazard which if not avoided will ...

Page 35: ...ions importantes relatives au produit dans ce manuel Ce symbole signale la présence d un danger d électrocution Risque de pincement Ces symboles vous avertit que les mains ou les doigts seront blessés sérieusement si vous les mettez entre les éléments en mouvement du mécanisme près de ces symboles Warnungen und Vorsichtshinweise Das Ausrufezeichen in Dreieck ist ein Warnzeichen das Sie darauf aufm...

Page 36: ... 465 3001 E mail IscoService teledyne com Advertencias y Precauciones Esta señal le advierte sobre la importancia de las instrucciones del manual que acompañan a este producto Esta señal alerta sobre la presencia de alto voltaje en el interior del producto Punto del machacamiento Sus dedos o manos seriusly serán dañados si usted los coloca entre las piezas móviles cerca de estos símbolos Table 1 7...

Page 37: ...on sequentially follow all instructions in sections 2 1 through 2 14 Note CombiFlash Rf PurIon system installation is not covered by this manual Instead refer to instruction sheet 60 5233 638 for the installation procedures Note Section 2 16 contains an Installation Qualification checklist If required sign off the checklist entries as you successfully complete the following sections 2 1 Unpacking ...

Page 38: ... Teledyne Isco or its authorized representative for advice Compare the contents of the boxes with the enclosed packing slips If there are any shortages contact Teledyne Isco immediately The fraction collector arm was stowed to prevent damage during shipping The arm stowing bracket should be removed at this time 1 Loosen the bracket s two thumbscrews along the sides of the arm Figure 2 1 Figure 2 1...

Page 39: ...environmental conditions and power requirements WARNING The system is heavy Use a two person lift to prevent injury Before making any connections to the CombiFlash Rf system place it on the bench or in the fume hood where it will be operated Temporarily position the system so you can access the back panels to complete the connections 2 3 Connect Power Ensure that the On Standby switch below the to...

Page 40: ...ms The black tubing P N 023 0503 06 is conductive This tubing is required to dissipate static electricity Figure 2 2 Recommended solvent connection 60 0923 017 Ferrule 60 0923 015 Compression Fitting Nut 60 5235 050 38 mm Cap or 60 5235 051 45 mm Cap 60 5234 129 Inlet Filter Assembly Place weighted filter at bottom of container To Solvent Level Sensing To Solvent Supply Connection ...

Page 41: ... or to change the B solvent mid run The accessory package includes several pieces to complete the solvent inlet connections To connect the solvent lines 1 Connect the solvent source to the system s Solvent Inlet ports Figure 2 2 shows the recommended connections when the user supplied solvent container has a 38 or 45 mm opening GL 38 or GL 45 If the container does not have a GL38 or GL45 opening d...

Page 42: ...fire ignited by electrostatic discharges Never substitute the black tubing on CombiFlash systems The black tubing P N 023 0503 06 is conductive This tubing is required to dissipate static electricity CAUTION Elevated flammable vapor levels are possible Ensure that the waste container is adequately ventilated preferably by placing it in a fume hood The system has two waste outlets on the back panel...

Page 43: ... Tubing Assembly 60 5235 053 38 mm Waste Cap or 60 5235 054 45 mm Waste Cap To Diverter Valve Waste Connection To Waste Level Sense Connection To Inject Valve Waste Connection Tubing Stop ferrule Ventilation Hole Luer fitting If necessary connect user supplied tubing and route to fume hood See Top View Top View Diverter Valve Waste Waste Level Sense Inject Valve Waste Ventilation about 2 inches 5 ...

Page 44: ...is ensures that the outlet is about two inches 5 cm below the container s maximum level Should the container not have a GL 38 or GL 45 opening omit the use of the waste cap Ensure the solvent tubes are secured so they drain into the waste container Secure the Waste Level Sense air tubing so its outlet is at least two inches 5 cm below the container s maximum level Seal the container opening to avo...

Page 45: ... and tubing clamps identified in figure 2 4 This releases the tubing lines for placement in the solvent supply and waste reservoirs Note Due to the large size of the inlet filter and inlet line tubing connections the tubing assemblies have been pre assembled with a bottle cap the is typical for the region GL 38 in the USA and GL 45 in the rest of the world If these caps aren t suitable for your co...

Page 46: ...t container level with or above the CombiFlash Rf system Placing solvent containers below the level of the system can contribute to decreased flow due to the high vapor pressure of DCM This problem becomes more pronounced as the ambient temperature increases 2 7 External Gas 2 7 1 CombiFlash Rf Rf Lumen and EZ Prep The CombiFlash Rf Rf Lumen and EZ Prep systems use an internal air pump to provide ...

Page 47: ... can deliver 2 5 SLPM at 60 to 70 psi 2 8 Connect and Route Drain Lines WARNING Risk of fire or equipment damage Failure to connect drain lines may allow organic solvents to pool in unsafe areas creating a potential for dangerous levels of flammable vapors Improper draining may damage the instrument s internal components The CombiFlash Rf system has drain tubes extending from its back panel The tu...

Page 48: ...he end of both drain tubes to a suitable waste fluid collection container Vacuum or pressurized air applied to the outlet end of the drain tube must exist at the collection tray drain hole Rf only Vacuum or pressurized air applied to the outlet end of the drain tube must exist at the top shelf drain hole ...

Page 49: ...rap must be filled with fluid to prevent sample loss To accomplish this raise the drain tubing above the instrument and place 10 mL of liquid such as isopropyl alcohol into the tube Lift it high enough so the fluid enters the P trap drain 6 Route the end of the P trap drain tube to a suitable waste fluid collection container Please be aware that as the tubing is lowered several ml of isopropyl alc...

Page 50: ... at least 3 cm 1 25 of air space behind it for ventilation Position the solvent and waste containers as necessary Note When using higher density solvents such as dichloromethane DCM place the solvent container level with or above the CombiFlash Rf system Placing solvent containers below the level of the Rf can contribute to decreased flow due to the high vapor pressure of DCM This problem becomes ...

Page 51: ...l tubes 150 60 5237 032 Two racks for 16 x 150 160 mm test tubes 18 mL Total tubes 150 60 5237 033 Two racks for 18 x 150 mm test tubes 25 mL Total tubes 140 60 5237 034 Two racks for 18 x 180 mm test tubes 30 mL Total tubes 140 60 5237 035 Two racks for 25 x 150 mm vials 50 mL Total vials 60 60 5237 040 One rack for twelve 480 mL French square bottles 60 5394 469 Two racks for 20 mL 28 x 61 mm sc...

Page 52: ...CombiFlash Rf User Manual 2 16 Figure 2 7 Loading test tubes ...

Page 53: ...ing outward and the rack is pushed in until it is seated When you turn the power switch to on the system will automatically detect the type of rack and configure program settings accordingly Later in section 2 13 6 you can configure the maximum volume for each tube size 2 11 External Detector Optional CombiFlash Rf systems with serial numbers greater than 209C20092 can be configured for use with a...

Page 54: ... To configure the system open the Configuration window by selecting Tools Configuration from the PeakTrak menu The configuration window has four tabs Instrument Configuration Network Configuration User Preferences and Prep HPLC on EZ Prep systems only Network Configuration settings are discussed later in Section 7 REMOTE INTERFACES Adjust the following sections 2 13 1 through 2 13 8 on the Instrum...

Page 55: ...olvent container and alerts you when there is not enough 6 If using the solvent level sensing feature enter the Minimum Solvent Level density dependent as a range in centimeters To understand this range consider that dichloromethane is more dense than hexane If the selected range is 2 4 the system triggers an alert when the dichloromethane level falls to about 2 cm above the weighted filter At the...

Page 56: ...vent unauthorized time changes this feature is password protected The system is shipped with the password set to combiflash Use the Tools Set Password menu command to change this password for greater security 2 13 5 Vapor Limit The system has an internal vapor sensor that detects vapors present in the immediate atmosphere When the limit is exceeded the CombiFlash Rf will shut down to avoid a hazar...

Page 57: ...hese values to set the desired default volume collected in each container Just be sure you don t overflow the containers by exceeding their capacity The system will automatically advance to the next tube when this default volume is met in each tube Keep in mind that advanced method settings discussed in Section 5 and the on line help may override this default setting During a run other factors suc...

Page 58: ...onnects the inflection points that define the gradient with a straight line Step The system holds each B value until it reaches the next programmed B Because the system holds the B values the changes at each new value are nearly instantaneous producing a stepped appearance on the plot area Isocratic The system holds the initial solvent mix for the entire run Figure 2 9 Gradient types Enable Run Le...

Page 59: ...nal minute At nine minutes a peak was eluting The system extended the run holding the B at the maximum level for another five minutes This also occurred at fourteen and nineteen minutes resulting in the second and third extensions At 24 minutes the B solvent strength returned to zero Before the final minute elapsed more compound was detected causing the system to extend the run for a final five mi...

Page 60: ... SIZE This data will be printed on the chromatograms for future reference 3 Enter a COLUMN DIAMETER This information will be used by the system to recommend an optimal flow rate to achieve highest resolution for the column being defined 4 Enter a COLUMN LENGTH This is used to recommend a separation length This length is based on a gradient segment approximately 12 column volumes in duration 5 Sele...

Page 61: ...e it 2 Place the Power switch below the LCD display in the Off position and wait one minute or more CAUTION Always wait until the screen turns off or at least one minute after placing the Power switch in the Off position Moving the switch to the Off position begins a power down sequence that takes up to one minute to complete If you move the switch to the ON position before the sequence is complet...

Page 62: ...e If you are performing an autoprime after redefining some of the solvents it may be beneficial to run 2 autoprime operations sequentially to get full flushing of the lines 3 Click the PLAY button to start priming the system Preparative HPLC systems typically require the user to open a prime valve and draw fluid with a syringe to prime the system The EZ Prep doesn t require this action due to its ...

Page 63: ...is also accomplished by performing the defined normal phase procedure below This tests all EZ Prep system functions also To do so use a pre packaged CombiFlash Rf test kit Part number 60 5237 050 Test kit containing five of the 5 gram size solid load cartridges pre filled with 0 5 grams of test sample NPHE and five 4 gram RediSep Rf silica gel columns Part number 60 5237 051 Test kit containing fo...

Page 64: ...mbiFlash Rf User Manual 2 28 2 16 Installation Qualification Checklist Table 2 1 may be completed to verify and document the installation procedures contained in Section 2 of this guide See following page ...

Page 65: ...NT LINES EXCLUDES EZ PREP 2 5 CONNECT WASTE LINES EXCLUDES EZ PREP 2 7 EXTERNAL GAS Optional 2 8 CONNECT AND ROUTE DRAIN LINES 2 9 POSITION THE SYSTEM 2 10 INSTALL COLLECTION TUBE RACKS 2 11 EXTERNAL DETECTOR OPTIONAL 2 12 TURN ON POWER 2 13 CONFIGURE THE SYSTEM 2 14 PRIME THE SOLVENT LINES 2 15 SYSTEM VERIFICATION Certification of Section 2 Completion Installer Name print Installer Signature Date...

Page 66: ...ated for operation with reagent grade solvents Operation at pressures 5 bar 75 psi with high purity hexanes 99 pure at 100 concentration may cause the pump to stall and produce a grating sound Many times normal operation can be restored by removing the high pressure load and flushing the pump with isopropyl alcohol 3 1 Unpacking the Unit The CombiFlash Rf 150 system is shipped in a single carton C...

Page 67: ...pare the contents of the box with the enclosed packing slips If there are any shortages contact Teledyne Isco immediately The fraction collector arm was stowed to prevent damage during shipping The arm stowing bracket should be removed at this time 1 Loosen the bracket s two thumbscrews along the sides of the arm Figure 3 1 Figure 3 1 Remove arm stowing bracket and spacer 2 Push the arm to the lef...

Page 68: ...the system on the bench or in the fume hood where it will be operated Temporarily position the system so you can access the back panels to complete the connections 3 3 Connect Power Ensure that the On Standby switch below the touch screen panel is in the Standby position Then use the supplied IEC power cord to connect the CombiFlash Rf to mains power WARNING Mains power must meet the voltage frequ...

Page 69: ...nt should be used The solvent should not contain any dissolved solids The CombiFlash Rf 150 system has two solvent inlet ports on the back panel one A solvent and one B solvent Figure 3 2 Figure 3 2 CombiFlash Rf150 solvent inlet ports The system requires at least one A and one B solvent to form a binary gradient It assumes that the B solvent is stronger than A When using the optional valve kit th...

Page 70: ...nd Solvent Inlet Filter assembly to the B Solvent inlet 3 Insert the filter end of each solvent inlet filter assembly into their respective solvent containers 4 The accessory package includes labels to easily identify the inlet lines Apply the A and B labels to the solvent lines above the solvent container openings CAUTION If solvent containers are reused particulate matter can accumulate in the c...

Page 71: ...levated flammable vapor levels are possible Ensure that the waste container is adequately ventilated preferably by placing it in a fume hood CAUTION Do not overfill the waste collection containers Regularly monitor and empty the bottles before they overfill The system has one waste outlet on the back panel Diverter Valve waste Accessory package P N 60 5239 012 includes a Waste Tube Assembly P N 60...

Page 72: ...bulkhead fitting This will seat the ferrule in the fitting 2 Route the tubing and insert the weighted end into the user supplied waste container 3 6 Connect and Route Drain Lines WARNING Risk of fire or equipment damage Failure to connect drain lines may allow organic solvents to pool in unsafe areas creating a potential for dangerous levels of flammable vapors Improper draining may damage the ins...

Page 73: ... drain by connecting a vacuum or air supply source to the outlet end of the drain tube Then verify the presence of such vacuum or air supply source on the drain Figure 3 5 3 Route the end of both drain tubes to a suitable waste fluid collection container Note It may be necessary to extend the drain tube If so splice the tubing with user supplied tubing The user supplied tubing should have an insid...

Page 74: ...at the CombiFlash Rf has at least 3 cm 1 25 of air space behind it for ventilation Position the solvent and waste containers as necessary Note When using higher density solvents such as dichloromethane DCM place the solvent container level with or above the CombiFlash Rf system Placing solvent containers below the level of the Rf can contribute to decreased flow due to the high vapor pressure of D...

Page 75: ...4 mL Total tubes 150 60 5237 031 Two racks for 16 x 125 mm test tubes 15 5 mL Total tubes 150 60 5237 032 Two racks for 16 x 150 160 mm test tubes 18 mL Total tubes 150 60 5237 033 Two racks for 18 x 150 mm test tubes 25 mL Total tubes 140 60 5237 034 Two racks for 18 x 180 mm test tubes 30 mL Total tubes 140 60 5237 035 Two racks for 25 x 150 mm vials 50 mL Total vials 60 60 5237 040 One rack for...

Page 76: ...tubes CAUTION Risk of broken glass or equipment damage Do not load test tubes longer than the length listed on the rack label 2 While holding the rack with the rack label visible Figure 3 7 insert the racks into the system Slide the rack in until you feel it drop into its seated position Figure 3 7 Inserting the collection tube rack Rack Label ...

Page 77: ...ence If grinding is heard there is a problem with the homing of the fraction collector arm Contact the factory for assistance 3 The system is ready for operation when the PeakTrak screen is displayed 3 10 Configure the System Before operating the system it should be configured for the desired operation To configure the system open the Configuration window by selecting Tools Configuration from the ...

Page 78: ...ry has more than one CombiFlash Rf system Time Zone Select your time zone from the drop down list box 3 10 3 Set Date Time Click this button to open a window from which you can set the system date and time To prevent unauthorized time changes this feature is password protected The system is shipped with the password set to combiflash Use the Tools Set Password menu command to change this password ...

Page 79: ...tration representing a safe setting but one with a reduced margin for error 3 10 5 Set Default Tube Volumes Click this button to open a window from which you can set the default volume of the collection tubes You can increase or decrease these values to set the desired default volume collected in each container Just be sure you don t overflow the containers by exceeding their capacity The system w...

Page 80: ...it takes to pump enough solvent to exchange the volume held by the column The duration in minutes will vary according to the column media and size and the flow rate Gradient Method Select the standard gradient type Figure 3 8 Linear The system gradually mixes solvents A and B from the last programmed B until it reaches the next programmed B This method connects the inflection points that define th...

Page 81: ...he Run Length Extension is enabled it will automatically extend the run one time to clear the column and plumbing of any remaining material Figure 3 9 Automatic Run Extension Examples Figure 3 9 illustrates the possible run extensions The original method was programmed to rise to the maximum B over seven minutes hold for two minutes and return to the minimum B for a final minute At nine minutes a ...

Page 82: ...ition and wait one minute or more CAUTION Always wait at least one minute after placing the Power switch in the Off position Moving the switch to the Off position begins a power down sequence that takes up to one minute to complete If you move the switch to the ON position before the sequence is complete the system may not start up correctly CAUTION Except during an emergency never remove AC power...

Page 83: ...ance to the next Auto Prime step you can click the Fast Forward button The Auto Prime window closes when finished After Auto Priming the system is ready for operation Section 5 Use the Auto Prime feature for quick solvent changes by pumping a fixed amount of solvent through the waste fluid path at a high flow rate For more advanced priming functions such as varying the flow rates fluid paths etc u...

Page 84: ...2 INSTRUMENT LOCATION 3 3 CONNECT POWER 3 4 CONNECT SOLVENT LINES 3 5 CONNECT WASTE LINES 3 6 CONNECT AND ROUTE DRAIN LINES 3 7 POSITION THE SYSTEM 3 8 INSTALL COLLECTION TUBE RACKS 3 9 TURN ON POWER 3 10 CONFIGURE THE SYSTEM 3 11 RESTART THE SYSTEM 3 12 SYSTEM VERIFICATION Certification of Section 3 Completion Installer Name print Installer Signature Date Operator Name print Operator Signature Da...

Page 85: ...CombiFlash Rf User Manual 3 20 ...

Page 86: ...following sections Note The optional 4x module is not compatible with the CombiFlash Rf 75 system 4 1 Unpacking the Unit The CombiFlash Rf 4x module is shipped in a single carton Carefully unpack the shipment and inspect the contents If there is any damage to the shipping carton or any components contact the shipping agent and Teledyne Isco or its authorized representative immediately WARNING If t...

Page 87: ... conditions and power requirements Before making any connections to the CombiFlash Rf 4x module place it on the bench or in the fume hood where it will be operated Temporarily position the system so you can access the back panels to complete the connections 4 3 Connect Power Ensure that the On Standby switch below the CombiFlash Rf system touch screen panel is in the Standby position Then use the ...

Page 88: ...d internal valves clean solvent should be used The solvent should not contain any dissolved solids The CombiFlash Rf system has four solvent ports on the left side panel To complete the solvent connections Figure 4 1 Labeled ports on CombiFlash Rf system side panel 4 4 1 Connecting the CombiFlash Rf with 4x Module 1 Remove the jumper tubing from ports A B C and D 2 Locate the solvent lines on the ...

Page 89: ... used as an example only Figure 4 2 Component arrangement for connection with Rf system 4x module and PurIon 2 Connect the 4x tubing to the Rf except for the tubing marked D according to CONNECTING THE COMBIFLASH RF WITH 4X MODULE 4 4 1 3 Connect the 4x tubing marked D to the shorter tubing assembly from the coupling package using the coupler as shown in Figure 4 3 4x module Rf PurIon ...

Page 90: ... to connect Waste Port tubing may allow organic solvents to pool in unsafe areas possibly creating dangerous levels of flammable vapors WARNING Risk of fire ignited by electrostatic discharges Never substitute the black tubing on CombiFlash systems The black tubing P N 023 0503 06 is conductive This tubing is required to dissipate static electricity CAUTION Elevated flammable vapor levels are poss...

Page 91: ... valve cleaning The Rf 4x module can automatically detect full waste bottles and stop operation to prevent overfilling a waste container This safety feature requires five air line connections one Waste Level Sense From Rf inlet to receive air or external gas from the CombiFlash Rf system four Waste Level Sense outlets 1 2 3 and 4 Note The following instructions assume that the waste from each chan...

Page 92: ...te Level Sense air The cap and black tubing from the Inject Valve Waste should remain attached to the waste bottle 2 At the CombiFlash Rf system back panel disconnect the black tubing from the Diverter Valve Waste port and the natural tubing from the Waste Level Sense port Note The Inject Valve Waste tubing must remain connected between the Rf system back panel and its waste container Refer to Fig...

Page 93: ...ten the threaded fitting 4 Locate the 20 inch 50 cm length of natural tubing from the accessory package Using nuts 60 0923 015 and ferrules 60 0923 017 connect this tubing between the CombiFlash Rf system s Level Sense port and the Rf 4x module s Waste Level Sense From Rf port Figure 4 6 CombiFlash Rf system to Rf 4x waste tubing connections all other connections not shown Waste Solvent Level Sens...

Page 94: ...f 4x module Column Waste connections 1 2 3 or 4 To Rf 4x Module Waste Level Sense connections 1 2 3 or 4 Channel 1 Only To Rf system Inject Valve Waste See step 8 for details on this connection for channels 2 through 4 Tubing Stop ferrule Ventilation Hole Luer fitting If necessary connect user supplied tubing and route to fume hood See Top View Top View Column Waste Waste Level Sense with tubing s...

Page 95: ...biFlash Rf system back panel the black tubing should still be connected to the Inject Valve Waste port from step 1 If not reconnect the tubing d At the waste container cap for channel 1 insert the black tubing into the Diverter Valve Waste opening e At the waste container cap for channel 1 insert the natural tubing into the Waste Level Sense opening Figure 4 7 Push the stop ferrule on the Waste Le...

Page 96: ...ckage and connect it to the Valve Waste Out bulkhead fitting on the Rf 4x module Route the other end of this tubing to one of the waste bottles The channel 2 waste bottle is shown in Figure 4 10 You can alternatively route it to a container other than those used for channels 2 through 4 however the system will not be able to detect the level and prevent overfilling To Waste Bottle 1 All other conn...

Page 97: ...re that waste containers are no more than 3 feet below the supply solvent levels Placing solvent containers above the system and waste containers on the floor may cause the internal check valves to open and allow solvent to flow through the system when in the standby state Note The Rf 4x back panel ports labeled A and B are not used To Waste Bottle 2 ...

Page 98: ...or can access all of the front view features and controls Figure 1 7 2 Position the Rf 4x module along the left side of the CombiFlash Rf system 3 The Rf 4x module has a tab extending from the right side of its base plate Slightly raise the CombiFlash Rf system and slide the Rf 4x module so that the system will rest on the module s tab The weight of the CombiFlash Rf system on the tab will hold th...

Page 99: ...tion The system will begin its startup routine which includes self diagnostics During the startup routine the system will detect the connected Rf 4x module and automatically configure the user interface to access the additional channels The system is ready for operation when the PeakTrak screen is displayed Thumbscrew one of three ...

Page 100: ...Tools Manual Control menu command 4 Select the Column 2 the channel option 5 Click the Prime B button The system pumps 100 solvent B through channel 2 Note When priming the first time inspect the solvent and waste connections to the system If any leaks are observed click the Cancel button to stop the pump Correct the leak by tightening the fitting an additional 1 4 turn and then restart the prime ...

Page 101: ... NPHE and five 4 gram RediSep Rf silica gel columns Part number 60 5237 051 Test kit containing four of the 25 gram size solid load cartridges pre filled with 0 5 grams of test sample NPHE and four 4 gram RediSep Rf silica gel columns Part number 60 5234 626 Test mixture supplied in the PurIon accessory kit containing 10 g of MSD test mix Part number 60 5234 315 Test mixture supplied with APCI pro...

Page 102: ...UNPACKING THE UNIT 4 2 INSTRUMENT LOCATION 4 3 CONNECT POWER 4 4 CONNECT SOLVENT LINES 4 5 CONNECT WASTE LINES 4 6 CONTROL CONNECTION 4 7 POSITION THE SYSTEM 4 8 REMOVE SHIPPING HARDWARE 4 9 TURN ON POWER 4 10 PRIME THE SOLVENT LINES 4 11 SYSTEM VERIFICATION Certification of Section 4 Completion Installer Name print Installer Signature Date Operator Name print Operator Signature Date Comments ...

Page 103: ...CombiFlash Rf User Manual 4 18 ...

Page 104: ... are not soluble in solvents that are compatible with the chromatography In addition the compounds may have very limited solubility in any solvent resulting in sample volumes that are impractical for good chromatography The answer in this case is solid sample introduction Here the reaction mixture or dissolved sample is mixed with the same media in the chromatography column Some samples of this ty...

Page 105: ... method such as rotary evaporation Alternatively you can dry the prepared cartridge after step 5 by drawing the solvent out using a vacuum or using the Rf system s air purge 3 Load the media and sample mixture into the cartridge Tap the cartridge on the bench top to settle the mixture 4 Place a frit on the top of the cartridge Force the frit down against the mixture using the plastic plunger 5 Wip...

Page 106: ...dges 60 5237 044 fits 32 and 65 gram solid load cartridges 2 Press the lever on the side of the cap and fully extend the plunger Figure 5 1 Figure 5 1 Press the lever and extend the plunger 3 Slide the plunger into the cartridge until it reaches the top frit Figure 5 2 4 Press the lever and push the cartridge into the cap Align the cartridge so that it fits fully into the recess in the cap Figure ...

Page 107: ...CombiFlash Rf User Manual 5 4 Figure 5 2 Insert the plunger to the bed Figure 5 3 Align and push cartridge into the cap and then rotate the cartridge to secure it 1 2 3 ...

Page 108: ... 1 for use on the CombiFlash Rf RediSep columns larger than 100 g meet Pressure Vessel Directive 97 23 EC Teledyne Isco strongly recommends against the use of columns rated less than 210 psi 1448 kPa Note For best results always use RediSep Rf columns The system will not automatically detect other columns The system also limits the maximum operating pressure to 50 psi when the column is not detect...

Page 109: ... Default methods are optimized for the use of RediSep Rf columns The default settings will collect all fluid in the fraction collector rack differentiate between UV 254 nm vs non UV absorbing fluid and place the fluids into separate tubes cut UV absorbing peaks based on slope detection or level threshold To start the run from the PeakTrak Main window 1 Enter a sample name If you choose not to Peak...

Page 110: ... if you have pre loaded the sample on the column The system will skip column equilibration so that the sample will not be flushed from the column before the run Loading Type options for the Rf 150 system are Equilibration Select this option if you intend to equilibrate the column before introducing the liquid or solid sample No Equilibration Select this option to skip column equilibration 5 Review...

Page 111: ... the P trap is full for maximum ELSD signal strength This can be done by lifting the drain line above the instrument and placing 10 ml of isopropyl alcohol in the drain line Lift the line sufficiently that the fluid flows into the P trap drain Then place into a waste container so that the excess fluid can drain out of the trap If you normally use higher boiling point solvents such as water the P t...

Page 112: ... system equilibrates the column and then waits When instructed perform the following steps a Place the injection syringe on the injection port b Slowly force the liquid into the injection port c Chase the first injection with a second injection solution of at least 0 25 mL The chase solution can be the starting mobile phase or diluted sample mixture d Click OK to continue the run PurIon Loading Pu...

Page 113: ...ient while monitoring the progress on the PeakTrak main window If desired gradient parameters may be modified during the run See the Real time Gradient Editing on line help topic As the run progresses the absorbance trace is drawn on the Gradient Plot area The separation or purification continues until the end of the run defined by the run length setting During the run data is automatically saved ...

Page 114: ...artridge with air purge enabled If you suspend the run with the Stop button do not remove the column and or solid sample cartridge without first pressing the Fast Forward button to purge solvents from all lines If you stop the run because your peak of interest has been collected protect the next user from being sprayed by solvents left in the lines by pressing Fast Forward so the instrument purges...

Page 115: ...on of this delay will vary with the flow rate Rewind This button is active when the system has completed the run or if the run was stopped by clicking the Stop button The Rewind button returns you to the Main window with the current method If you have stopped the run before its programmed run length has elapsed clicking the Rewind button changes the current method to the new shorter run length Thi...

Page 116: ...e the Rf of the slowest eluting compound of interest The Rf should be between 0 2 and 0 8 the same range used by the Gradient Optimizer 6 3 3 Note the Percent B solvent used to run the TLC plate If a compound displays tailing peaks as streaks on TLC the Rf used corresponds to the bottom of the streak 2 Load the Sample in the Solid Load Cartridge and note the cartridge size Refer to list below to d...

Page 117: ...un the flow rate dropped to 30 mL min The equation is then T 45 mL 0 35 30 mL min 4 3 minutes In this example the Cartridge Bypass feature was used 4 3 minutes after the solvent gradient reached 30 B The calculation is conservative but allows you to minimize the time needed to keep the solid load cartridge in the fluid path 5 4 3 About Solvent Level Detection When enabled in the TOOLS Configuratio...

Page 118: ...ficient the system displays the alert message again Ignore This option is available when the estimated usage rates indicates that the solvent levels are insufficient Select Ignore to clear the message and continue the run The system then ignores the estimated solvent usage rate for the remainder of the run but continues to measure the solvent level Should the level become insufficient the system w...

Page 119: ...mn 1 Remove the union installed on the preparative column tubing on the right side of the instrument 2 Take the tubing supplied with the guard column and connect it to the guard column outlet 3 Connect the line that exits from the prep inject valve to the guard column inlet 4 Remove the cap on top of the column mounting tower by grasping the tabs on the front and back of the cover 5 Place the guar...

Page 120: ...ample should be similar to the stating conditions of the gradient if possible If the sample is dissolved in a solvent that is too strong it can have negative effects on the chromatography The sample should be filtered with a 2 µm filter or finer to prevent clogging of the HPLC column The loop will contain solvent from the previous separation Typically reverse phase separations end with an organic ...

Page 121: ...umn or select Flash Column to return to flash operation 3 The sample loading technique must be selected LOAD NOW assumes that your sample is ready for loading If that is correct inject the sample into the HPLC inject port Remember that the sample volume should not exceed of the loop volume 4 Then press the sample loaded button to start the separation If LOAD AFTER EQUILIBRATION is selected the STA...

Page 122: ...on number in brackets Some topics are only available in the on line help format 6 1 PeakTrak Overview PeakTrak is the control software for Teledyne Isco s CombiFlash Rf system This overview provides a description of The PEAKTRAK WINDOW ELEMENTS 6 1 1 The METHOD FILE 6 1 2 The RUN FILE 6 1 3 HOW TO GET PEAKTRAK HELP 6 1 4 6 1 1 PeakTrak Window Elements The MAIN WINDOW 6 3 1 displays the current MET...

Page 123: ...Method file The system uses the method file to direct the system operation after you click the Play button PeakTrak categorizes the method settings as Basic or Advanced Basic settings are the frequently used controls accessed through the MAIN WINDOW 6 3 1 Use the METHOD EDITOR 6 3 2 window to access the Advanced settings Method files are stored by the system and can be opened for review reuse or m...

Page 124: ...ged to meet your specific requirements See EDITING A DEFAULT METHOD 6 4 4 6 1 3 Run File When the system has finished a run it saves the run history in a Run file The history includes the METHOD FILE 6 1 2 settings rack and tube information spectral data and a chromatogram You can open and review the Run files stored by the system To open a Run file use the FILE OPEN 6 2 1 2 menu command Run files...

Page 125: ...Copy or Move files to flash drive option To remove a file from the internal hard drive highlight the file or enter the filename and click the Delete button To remove multiple files click the Delete by Age button Then specify the age limit in months and click OK Use the Move and Delete options with caution as the files cannot be recovered from the internal hard drive once the action is complete 6 2...

Page 126: ...aves a new method file with the gradient and run length scaled to the selected column size 6 2 1 7 Save Run As PDF Choose this command to save the displayed run on a remote computer s hard drive or a USB Flash storage device connected to the system When selecting this menu command from the touch screen the system saves the file on the USB storage device The default file name will be the same as th...

Page 127: ... the touch screen this command opens the FILES 6 3 6 window so you can save the file on a USB Flash storage device When selecting this command from a remote computer PeakTrak displays a window from which you can save the method file 6 2 1 11 Export SMM XL Method Choose this command to export a method file for use on a CombiFlash Companion system equipped with the Solvent Management Module SMM or a...

Page 128: ...rowser ION FINDER Enables the user to find fragments and adducts based on the molecular weight of their desired compound DESIRED MASS enter the molecular weight of your compound rounded to the nearest integer DETECTION IONS list of ions to be detected Detection Ion list of possible adducts or fragments based on the value entered in the desired mass control and detected by the system Checking one o...

Page 129: ...n the PurIon mass spectrometer for maintenance or to move the system WARNING Warning Do not shut down or disconnect the vacuum line to the roughing pump until the PurIon is fully vented as indicated by PeakTrak 6 2 4 Tools PeakTrak s Tools menu has the following options 6 2 4 1 Auto Prime Valve Wash Choose this command to automatically prime the solvent pumps On CombiFlash Rf systems this feature ...

Page 130: ...to open the SET ADMINISTRATOR PASSWORD 6 3 14 window Passwords protect unauthorized modifications to Default methods User management system date and time system password Before any of the above can be accessed the user must enter a password Password protection for the default methods can be disabled so all users can modify default methods 6 2 4 7 User Management Choose this command to open the USE...

Page 131: ...ns 6 2 5 1 Help Choose this command to view the Help documentation 6 2 5 2 Service Qualified service personnel use this command to access the system s service functions These service functions are password protected to restrict their use to only trained personnel 6 2 5 3 Software Update Choose this command to open a window used to install patch files to update your CombiFlash Rf system software 6 ...

Page 132: ...will find information on the following MAIN WINDOW 6 3 1 METHOD EDITOR 6 3 2 GRADIENT OPTIMIZER 6 3 3 COLUMN DATA 6 3 4 BATCH 6 3 5 FILES 6 3 6 SET DATA PATH 6 3 7 MS METHOD DEVELOPMENT 6 3 8 MS MANUAL CONTROL 6 3 9 IONIZATION SETTINGS 6 3 10 AUTO PRIME VALVE WASH 6 3 11 MANUAL CONTROL 6 3 12 CONFIGURATION 6 3 13 SET ADMINISTRATOR PASSWORD 6 3 14 USER MANAGEMENT 6 3 15 6 3 1 Main Window The Main w...

Page 133: ...g or selecting the Run Length The left Y axis displays absorbance units and the right Y axis indicates the percentage of solvent B By default PeakTrak automatically scales the left Y axis to best display the absorbance trace PeakTrak also sets the right Y axis to 100 You can override the Y axes scales by clicking the Format Graph button and setting the desired values The Cartridge Bypass button ma...

Page 134: ...creen Up to 4 spectra can be saved in a run report The button depicted with a triangle pointing down allows a user to cycle through saved spectra The UV UV vis on Rf systems with a UV vis detector button displays the UV spectrum on CombiFlash systems This spectrum hides the flow rate and solvent selection controls Pressing the UV control again causes the spectrum to disappear When the spectrum is ...

Page 135: ...em sets the flow rate to the optimum flow rate of the column Detector Rf systems including those equipped with 4x Reports the current peak detection mode To change the peak detection settings open the METHOD EDITOR 6 3 2 window Solvent A Select the desired solvent from the list The solvents in the list are those defined by the CONFIGURATION 6 3 13 window For assistance in selecting a solvent see t...

Page 136: ...d the run or if the run was Stopped by clicking the stop button The Rewind button returns you to the MAIN WINDOW 6 3 1 If you have stopped the run before its programmed run length has elapsed the current method is modified using the new run length This modified method is ready for the next run or can be saved for future runs Fast Forward Click this button to jump to the next step of a run Once you...

Page 137: ...impurities The peak collection data is displayed on the left side of the Main window Rack and tube information Collected peaks are color coded in the rack diagram so that you can easily locate the peaks of interest The tube colors correspond to the color bars under the peaks displayed on the chromatogram If during the run more than one set of tube racks was filled use the Next and Previous Rack bu...

Page 138: ...e system s internal hard drive Save Click this button to save any modifications to the current method file Note that if you attempt to save modifications to a default method file the FILES 6 3 6 window will open instead so you can rename the file This preserves the default method If you do wish to edit and save the system s default methods use the TOOLS EDIT DEFAULTS 6 2 4 4 command instead Save A...

Page 139: ... are reserved by the operating system etc If you do not type a Sample Name PeakTrak will generate a date time stamp for the name when you click the Play button to begin the run Flow Rate Type or select the desired flow rate for the run When using the Isco default column methods the system sets the flow rate to the optimum flow rate of the column Equilibration Volume Type or select the volume of so...

Page 140: ...sufficient post run air purge ensures that it will be empty To disable the air purge enter a value of 0 zero A column can also be manually air purged See MANUAL CONTROL 6 3 12 6 3 2 3 Run Notes Use this text entry box to enter comments or notes for the run These comments will be saved with the run and will appear in TXT and PDF reports 6 3 2 4 Gradient Plot Area The gradient plot area depicts the ...

Page 141: ...ed by the CONFIGURATION 6 3 13 settings Solvent B Select the desired solvent from the list You can program mid run solvent B changes by clicking the Edit Gradient button to open the GRADIENT TABLE Edit Gradient Although the gradient may be edited directly within the plot area you can also edit the gradient in tabular form Click this button to open the GRADIENT TABLE On Rf systems including those e...

Page 142: ...action collection tubes during a run Peaks Click this button to collect only eluted peaks in the fraction collection tubes during a run None Click this button to divert all fluids during a run to the waste port Tube Volume You can also specify the Tube Volume for collected fluids This volume can be the default maximum volume Max option as entered in the CONFIGURATION 6 3 13 window or a method spec...

Page 143: ...e or select the peak detection wavelength in nanometers then click the Details button to configure additional settings described below Slope Based Select this option to enable Slope based peak detection When enabled peaks will be recorded if the slope algorithm indicates a peak within the Peak Width setting Peak Width Select the average peak width setting Peak widths are measured at the baseline T...

Page 144: ...in 1 and 2 above Peak width is used to determine solvent suppression Peaks that are twice the peak width are deemed to be solvent or other baseline drift and the signal will be rezeroed Additionally you can type or select the minimum and maximum wavelengths limits in nanometers Mass Spectrometer Enable this option to monitor or detect compounds with a PurIon mass spectrometer system PurIon systems...

Page 145: ...led click the Details button to configure additional settings Signal Gain You may modify the gain to scale the detector signal Slope Based and Threshold Refer to these features described in 1 and 2 above Spray Chamber Temperature The default settings are 30 C normal phase default methods and 15 C reverse phase This setting may be adjusted from 10 to 60 C so that detection can be optimized for the ...

Page 146: ...em may automatically extend the isocratic hold during the run to increase peak resolution To open the Gradient Optimizer window open the METHOD EDITOR 6 3 2 window then click the Gradient Optimizer button 6 3 4 Column Data Rf systems including those equipped with 4x The Column Data window reports information about the RediSep Rf column installed in the system Compatible RediSep Rf and RediSep Rf G...

Page 147: ...n Type a unique descriptor PeakTrak saves the run information under this name Therefore PeakTrak cannot accept any characters that are reserved for the operating system etc If you do not type a Sample Name PeakTrak will generate a date time stamp for the name when you begin the run RediSep Select the column that will be used for the run See also COMBIFLASH RF COMPONENTS ON LINE Loading Type Select...

Page 148: ...o paste a file from the clipboard memory If the file already exists in the current folder the system will ignore the Paste command to prevent the original file from being overwritten Delete Click this button to delete a highlighted file or a folder and its contents New Folder Click this button to create and name a new folder Up Click this button to browse the contents of the next higher folder lev...

Page 149: ... if additional compounds of interest might be left on the column Load Previous Run from Detected Rack Rf and Rf Lumen This option appears when using the FILE OPEN 6 2 1 2 command If you click this option the system reads the RFID tag on a single rack and displays the RUN FILE 6 1 3 This feature is useful when there is a need to recall run results at a later time Cancel Click the Cancel button to c...

Page 150: ...nables a user to test and verify ionization conditions for their compound This command is not available from a remote connection This window contains the following controls POLARITY On the PurIon system this control changes the probe polarity between positive and negative ionization On PURION S and PURION L systems this button toggles the displayed mass spectrum between positive and negative ioniz...

Page 151: ... of the injection valve Filter the sample with a 0 45 µ filter to avoid clogging the PurIon tubing and probe capillary Sample concentration should be less than 20 µg mL FORMAT GRAPH Set the displayed range of the mass spectrum The PurIon system still collects the entire mass range even when the range is set within than the minimum and maximum values allowed for the spectrometer Values can range fr...

Page 152: ...mp open the priming valve on the fluid interface counterclockwise Use the 5 mL Luer lock syringe provided with the accessory kit to draw liquid into the pump Repeat this procedure once more to completely fill or purge the line from the carrier solvent reservoir to the priming valve Make sure the priming valve is tightly shut after priming the system STOP CARRIER PUMP Stops the carrier pump This ch...

Page 153: ...tion should be less than 20 µg mL POLARITY switches the mass spectrometer between positive and negative polarity FORMAT GRAPH Set the displayed range of the mass spectrum The PurIon system still collects the entire mass range even when the range is set within than the minimum and maximum values allowed for the spectrometer Values can range from 50 to 1200 Da PURION and PURION S or 2000 Da PURION L...

Page 154: ... software will change the labels on the control to reflect the probe installed in the mass spectrometer GAS TEMP the temperature of the nebulization gas for the probe Lower temperatures are used for more delicate heat labile compounds The temperature is set to quickly evaporate the carrier solvent note that PURION S and PURION L systems will display a single temperature for both positive and negat...

Page 155: ...r the starting mobile phase of the next run The Auto Prime window is opened by selecting the TOOLS AUTO PRIME VALVE WASH 6 2 4 1 menu command The window contains the following controls Progress bar This bar displays how much of the solvent has been pumped Solvent Selections There are 4 solvent selection lists labeled from 1st solvent through 4th solvent describing the order in which solvents will ...

Page 156: ...entage Solvent B type or select the mixture percentage Flow Rate Type or select the pump s flow rate in mL min Pump into Tube As a default setting solvent is pumped to the waste port during manual control If you would like to collect the solvent in a tube select the option button and enter the tube number This function cannot be used with the Waste Flow Path valve position This feature can be usef...

Page 157: ...cteristics of your CombiFlash Rf system It also allows you to configure the system for network connections for remote access and printing Open the Configuration window by selecting the TOOLS MANUAL CONTROL 6 2 4 2 menu command The configuration window displays three tabs INSTRUMENT CONFIGURATION 6 3 13 1 NETWORK CONFIGURATION 6 3 13 2 and USER PREFERENCES 6 3 13 3 6 3 13 1 Instrument Configuration...

Page 158: ...e triggered when the hexane solvent level falls to about 2 cm above the weighted filter CombiFlash Rf Name Enter a name for the system This name will appear in the title bar of the Main window The name will also appear in run summaries Unique names are helpful when operating more than one system Time Zone Select your local time zone Set Date Time Click this button to set the date and time From the...

Page 159: ...OADING A COLLECTION RACK ON LINE Enable Automatic Column Purchase This feature requires a current subscription in a Teledyne Isco Column Plan Contact your sales representative for more information on this feature The certificate issued with the column plan includes instructions for activating this feature TEST CONNECTION is used if a column plan is enabled and the system reports column usage via a...

Page 160: ... number The printer type either Postscript or PCL When this information is known you can proceed with configuring system for network printing Follow the on screen instructions for entering the address queue and printer type information After successfully printing a test page the network printer will be available for printing using the FILE PRINT 6 2 1 12 menu command and the AUTOMATICALLY PRINT RE...

Page 161: ...gram settings and chromatogram displays The duration in minutes will vary according to the column media and size and the flow rate Enable Run Length Extensions When enabled this option automatically extends the run if a peak is eluting at the end of the programmed run length This ensures that a late eluting peak is still collected Gradient Method Select the desired gradient method option If the Li...

Page 162: ...ommand is used to enter and change the system password and to enable password protection for the default methods To enter or change a password 1 Type the password The factory default password is combiflash 2 Type the password again to verify your entry 3 To protect the Default methods select the Require Password For Editing Default Methods option 4 Click the OK button to save your settings and clo...

Page 163: ...EEN when the cursor displays at a significant location from where the screen in touched A stylus should be used for this procedure for best accuracy A dialog will appear providing further directions Use the CANCEL button to cancel the calibration and the CALIBRATE button to start the calibration procedure Note once touchscreen calibration is started it must be completed or the touch screen may be ...

Page 164: ...nter the date and time as the sample name when you start the run 2 Review the PeakTrak Main window settings If you want to change any settings refer to the Editing a Method on line help topic 3 Click the Play button 4 Select the sample Loading Type from the list The Loading Type should support the sample injection technique you intend to use see SAMPLE INJECTION METHODS ON LINE Possible sample loa...

Page 165: ...r update the Start Rack and Start Tube 6 Review the Minimum Run Requirements The system will report the estimated solvent volumes expected waste collection tube usage etc You can use this information to verify that there will be enough solvent to complete the run the waste volume does not exceed the collection container s capacity and whether or not more tubes will be required during the run Note ...

Page 166: ... PURION S and PURION L systems only the ions may be a mix of positive and negative 11 Click OK and the run begins The system responds according to the sample Loading Type you selected in step 4 Rf systems including those equipped with 4x If you selected Solid Pause the system equilibrates the column with the starting B and then waits while you prepare the solid sample load cartridge Place the cart...

Page 167: ...s on the PeakTrak Main window If desired gradient parameters may be modified during the run See REAL TIME GRADIENT EDITING 6 4 6 As the run progresses the absorbance trace is drawn on the Gradient Plot area The purification continues until the end of the run defined by the run length setting See Also REDISEP RF COLUMN SELECTION GUIDE ON LINE SOLVENT SELECTION ON LINE EDITING A METHOD 6 4 2 EDITING...

Page 168: ...FIGURATION 6 3 13 window 6 4 2 2 Advanced method settings The METHOD EDITOR 6 3 2 window gives you access to advanced settings such as equilibration volume initial waste air purge peak detection and peak collection mode Equilibration Volume Column equilibration is optional but you may find that separations are more effective if the column is equilibrated before injecting the sample The recommended...

Page 169: ...present If you select All the module will collect all fluid during the time window regardless of the peak state Define up to three time windows Air Purge You can program the system to purge the column with air after a run This feature allows you to remove solvents from the column before it is discarded Enter the desired time to purge the column in minutes To disable the post run air purge enter ze...

Page 170: ...en an option is enabled the window also allows you to modify the setting details for that peak detection option All enabled options will be displayed on the chromatogram The options and settings for the Rf systems including those equipped with 4x are described below Note Note You can select up to four peak detection options excluding the External option on the Rf systems including those equipped w...

Page 171: ...m will cut a peak when either the Slope condition is true or when the Threshold condition is true Monitor Enable this option to only use the detection source as a monitor When enabled the detection source will be displayed as a trace on the gradient plot area but will not be used to cut peaks All Wavelength Detection Enable this option to detect peaks within a user selected range of wavelengths Wh...

Page 172: ...s setting is limited to a minimum of 5 C below the ambient temperature Drift Tube Temperature The default settings are 60 C normal phase default methods and 60 C reverse phase This setting may be adjusted from 30 to 90 C but is limited to a range of 5 C below and 60 C above the ambient temperature Mass Spectrometer PurIon systems only Enable this option to monitor or detect compounds with a PurIon...

Page 173: ... based and peak width options These are described in 1 and 2 above Rf150 systems with the variable wavelength option include a control to type or set the detection wavelength 6 4 2 3 Saving Changes to the Method File After you have edited the method file you can save the changes for future use Click the Save As button give the method file a descriptive name then click the Save button The method fi...

Page 174: ...the Scale option then choose the new column size and click the Save button The system will create a new method file with the gradient and run parameters scaled to the new column size This feature is useful when developing methods using small sample volumes After you optimize the method to successfully extract the compounds of interest you can then scale up the method to load and extract larger vol...

Page 175: ...Alternatively you can modify add insert and delete points using a tabular view on the Method Editor window Click the Edit Gradient button to open this view then use the controls to modify the settings Click the Edit Gradient button again to close the table view The system can also optimize a gradient from your TLC results To use this feature select a single solvent system and run two TLC plates ea...

Page 176: ...load cartridge too soon during the purification run may leave desired compounds on the solid load cartridge After removing the cartridge from the fluid path these compounds cannot be purified If you need to use this feature perform the following to ensure that you do not leave desired compounds on the cartridge 1 Run a TLC plate prior to starting the run Measure the Rf retention factor of the slow...

Page 177: ...ridge and you can safely click the Cartridge Bypass button For example a TLC plate run at 30 B revealed that the last desired compound had an Rf factor of 0 35 An empty 25 gram size solid load cartridge was filled with sample adsorbed onto 10 grams of silica and then placed on the system The programmed flow rate was 60 mL min During the run the flow rate dropped to 30 mL min The equation is then T...

Page 178: ...eparation you are also able to eliminate the time required for column equilibration after a gradient separation 6 4 9 Monitoring the Purity Measure When using two wavelength detection options a ratio of the two wavelengths can also be displayed which at times can provide the best indication of compound purity Refer to the following discussion If a pure compound is eluting the absorbance is linearl...

Page 179: ...oesn t will fail on saturated peaks flat on top due to detector saturation To display the ratio open the METHOD EDITOR 6 3 2 window and select the Show Ratio option 6 4 10 Viewing runs After completing a run the PeakTrak Main window is used to display all collected run data You can also open previous runs to view the chromatogram and the peak tube locations To open a previous run 1 From the main w...

Page 180: ...ewing the run from a remote personal computer the summary can be saved to any connected storage device If you are attempting to save a PDF file from the touch panel display insert a USB Flash drive in the USB port below the display panel Save As TXT Click this button to save the run summary in an ASCII text file format When viewing the run from a remote personal computer the summary can be saved t...

Page 181: ...wing the run 6 4 10 1 General instructions for reading the data Most elements on the window are color keyed to help you locate the tubes containing the peaks of interest Below each collected peak there is a color bar that matches a tube in the map on the left The tube map provides a visual representation of the tubes that contain the peaks of interest If you wish to identify the tube by number ref...

Page 182: ...eshooting To manually control the CombiFlash Rf system first open the MANUAL CONTROL 6 3 12 window by clicking the Tools Manual Control menu command 6 4 11 1 Pumping Solvents To pump either solvent select the solvent from the Solvent A or Solvent B lists Then click the Prime A or Prime B buttons to pump the selected solvent To pump a mixture or Solvent A and B adjust the Percentage Solvent B setti...

Page 183: ...impaired The system can be operated although the absorbance trace might appear noisy Yellow might be a normal indication for systems with flow cell windows stained by compounds Red lamp energy is obstructed to a degree that the system might not reliably detect peaks If you attempt to operate the system peak collection will be forced to collect all This prevents diverting desired compounds to waste...

Page 184: ...aboratory and the instrument Ensure that no open containers or spills of organic solvent are in close proximity to the system Ensure that the system is located in a well ventilated area Ensure that there is no visible solvent leakage from the system If PeakTrak continues to display the Vapor Limit alarm after you have made these checks and corrected any problems found it is likely that organic vap...

Page 185: ...CombiFlash Rf User Manual 6 64 ...

Page 186: ...department before proceeding The system has a factory assigned IP address 192 168 1 51 In many cases this address must be reconfigured for use on a corporate network To reconfigure the IP address 1 From the touch screen panel select the Tools Configuration menu command 2 Select the Network Configuration tab 3 Select Static IP as the Network Type Note The CombiFlash Rf system also provides limited ...

Page 187: ...features such as network printing Section 7 1 2 and network file saving Section 7 1 3 Networks with Wi Fi access points may also support remote control with mobile digital devices Section 7 1 4 7 1 1 Network PC Access A successfully networked CombiFlash Rf system can be accessed by a PC that meets the recommendations listed in Table 7 1 Table 7 1 Personal Computer Recommendationsa Operating System...

Page 188: ...ck OK to save the settings The CombiFlash Rf system will send a test page to the printer After successfully printing a test page the network printer will be available for printing using the File Print menu command or through the Automatically Print Report at End of Run option on the Tools Configuration User Preferences tab 7 1 3 Network File Save Configuration By default this option is disabled an...

Page 189: ...n 7 1 5 Install and Configure the PeakTrak App 1 From the Apple mobile digital device visit the App Store and locate the PeakTrak app by Teledyne Isco Note The App Store requires an Internet connection on the Apple mobile digital device 2 Install the app on the Apple mobile digital device 3 Open the PeakTrak app 4 From the PeakTrak display tap the button 5 Enter a descriptive name for the CombiFla...

Page 190: ...ctions may require a user account with Administrator privileges on the PC If you cannot modify the settings in sections 7 2 1 through 7 2 4 contact your Information Technology department 7 2 1 Windows 7 Settings 1 From the Windows Start menu select Control Panel then select the Network and Sharing Center option The PC displays the Network and Sharing Center 2 Select the Change Adapter Settings opt...

Page 191: ...settings now 5 Select the Use the following IP address option 6 Enter the IP address 192 168 1 200 7 Enter the Subnet Mask 255 255 255 0 8 Click the OK button to close the Internet Protocol Version 4 TCP IPv4 Properties window Click the OK button to close the Local Area Connection properties window 9 Shut down the PC and place the CombiFlash Rf system in Standby Figure 7 1 Local Area Connection Pr...

Page 192: ...he Local Area Connection icon and select the Properties option After you provide permission to continue the PC displays the Local Area Connection Properties window Figure 7 1 4 Select Internet Protocol Version 4 TCP IPv4 then click the Properties button The PC displays the Internet Protocol Version 4 TCP IPv4 Properties window Figure 7 2 Note If the Internet Protocol Version 4 TCP IPv4 option is n...

Page 193: ...ernet Protocol TCP IP settings now 5 Select the Use the following IP address option 6 Enter the IP address 192 168 1 200 7 Enter the Subnet Mask 255 255 255 0 8 Click the OK button to close the Internet Protocol Version 4 TCP IPv4 Properties window Click the OK button to close the Local Area Connection properties window 9 Shut down the PC and place the CombiFlash Rf system in Standby ...

Page 194: ...e 7 3 4 Highlight the Internet Protocol TCP IP item in the list and click on the Properties button Refer to Figure 7 4 5 Select the Alternate Configuration tab Click the User Configured option See Figure 7 5 6 Enter the IP address 192 168 1 200 7 Enter the Subnet Mask 255 255 255 0 8 Click the OK button to close the Internet Protocol properties window Click the Close button to close the Local Area...

Page 195: ...CombiFlash Rf User Manual 7 10 Figure 7 4 Local Area Connection Properties Figure 7 5 Alternate Configuration Settings ...

Page 196: ...em in the list and click on the Properties button The Internet Protocol Properties Window will open Figure 7 7 Note The following steps change the local area connection settings If the PC must be restored to its original network configuration record the present Internet Protocol TCP IP settings now 5 Click the Use the following IP address option 6 Enter the IP address 192 168 1 200 7 Enter the def...

Page 197: ...CombiFlash Rf User Manual 7 12 Figure 7 6 Local Area Connection Properties Window Figure 7 7 Internet Protocol Properties Window ...

Page 198: ...ing instructions Abbreviated instructions can be found in Section 5 of this guide 7 3 Direct Printing The CombiFlash Rf system supports direct printing to a USB printer The printer must support postscript To set up the printer 1 Connect the printer with the USB cable to the USB port on the back panel of the system 2 Select the Tools Configuration menu command 3 Select the Network Configuration tab...

Page 199: ...CombiFlash Rf User Manual 7 14 ...

Page 200: ...tion the CombiFlash Rf system so that the power cord can be unplugged or use a power strip where the plug can quickly be removed from the outlet in the event of an emergency When you first place the system in Standby internal components continue to operate for almost one minute while performing file maintenance and preparing the system for possible power removal CAUTION Removing the AC mains power...

Page 201: ...s from the column internal tubing and flow cell Refer to section 8 5 1 Allow Cone wash to run to completion PurIon systems only to wash residual compounds from the fluid interface probe and to clean the cone area Monthly Perform these tasks at least monthly more frequently if conditions warrant Tubing Inspection section 8 4 Collection rack and tray cleaning section 8 3 1 Monthly flow cell cleaning...

Page 202: ...Section 8 Maintenance 8 3 CAUTION Do not immerse the instrument in a water bath or subject it to a liquid spray The instrument is not watertight and these actions could damage the internal electronics ...

Page 203: ...yl alcohol 8 4 Tubing Inspection WARNING Risk of fire or equipment damage Faulty tubing fittings and drains may allow organic solvents to pool in unsafe areas creating a potential for dangerous levels of flammable vapors Improper draining may damage the instrument s internal components Perform a tubing inspection monthly 1 Visually inspect the solvent waste and drain tubing The tubing must be free...

Page 204: ...hole Figure 8 2 Top shelf drain hole Vacuum or pressurized air applied to the outlet end of the drain tube must exist at the collection tray drain hole Vacuum or pressurized air applied to the outlet end of the drain tube must exist at the top shelf drain hole ...

Page 205: ...se residual compounds to build up and crystallize which might result in cross contaminating later separation runs higher operating pressures reduced flow cell lamp energy a noisy baseline on the absorbance trace frequent messages recommending flow cell cleaning Figure 8 4 Typically chemists Stop and then Fast Forward the run after the last compound elutes This action skips the post separation flus...

Page 206: ...se containing more than 20 methanol with ammonia 8 5 2 Quick Cleaning when Recommended When the lamp energy is lower than normal the system will recommend flow cell cleaning Figure 8 4 before starting a separation run Figure 8 4 Flow cell cleaning message When the system displays this message you can Cancel Run recommended Click the Cancel Run button so you can perform a quick cleaning described i...

Page 207: ... will be forced to collect all This prevents diverting desired compounds to waste Yellow lamp energy is partially obstructed and the peak detector performance might be impaired The system can be operated although the absorbance trace might appear noisy Yellow might be a normal indication for systems with flow cell windows stained by compounds Green lamp energy is sufficient to detect peaks up to 2...

Page 208: ...ded solvent is the highest polarity solvent you have recently used solvent B 8 Monitor the Raw Lamp Energy gauge As the system pumps solvent the raw lamp energy should gradually improve Pump solvent for two to five minutes or until the indicator reaches the far right of the green range When the indicator is in the yellow the lamp energy and flow cell are ready for the next run However continuing t...

Page 209: ...e Dichloromethane DCM Effective at solubilizing organic molecules Dimethylsulfoxide DMSO Strong solvent that will clear organic sample Dimethylformamide DMF Strong solvent if other solvents do not produce the desired results Tetrahydrofuran THF Strong solvent Water DMF methanol A 50 25 25 solvent mixture effective in clearing some obstructions Water DMF Acetic Acid 30 30 30ml solvent mixture effec...

Page 210: ...methanol acetone or a strong solvent that readily dissolves residual sample material 7 Click the Prime B button to pump 100 Solvent B through the bypass tube and into the collection tubes 8 After three minutes click the Stop button Allow the system to stand for at least six hours Overnight is recommended 9 Return the B1 solvent line to the original solvent container 10 Perform the Quick Cleaning a...

Page 211: ...eplacement 1 Insert the ESI probe into the source chamber ensure the corona discharge pin is removed from the source chamber Refer to Removing the Ion Source Chamber and Reinstalling the Ion Source Chamber to remove the corona discharge pin APCI equipped systems only 2 Push down on the ESI probe and tighten the thumb screw on the ion source chamber to ensure the ESI probe is fixed in position Note...

Page 212: ...not twist 2 Unscrew the 10 32 PEEK fitting from the probe inlet 3 Disconnect the 1 8 PTFE tubing from the push to connect fitting labeled as Neb Gas 4 Disconnect the 1 8 PTFE tubing from the push to connect fitting labeled as APCI heated gas 5 Loosen the thumbscrew on the front of the ion source housing 6 Carefully lift and pull out the APCI probe from the source chamber 7 If changing to ESI remov...

Page 213: ...E tubing labeled Neb Gas into the push to connect fitting labeled as Neb Gas 5 Connect the 1 8 PTFE tubing labeled APCI to the push to connect fitting labeled as APCI heated gas 6 Finger tighten the 10 32 PEEK fitting 7 Connect the high voltage connector 8 6 5 Removal of Ion Source Housing 1 Follow the steps in Removing the ESI Probe or Removing the APCI Probe as appropriate to disconnect the line...

Page 214: ... source housing on top of the base plate and line up with the rear electrical connection Push down until source chamber is seated evenly across the base plate 2 Lock down two housing clamps at both sides 3 Finger tighten the 28 PEEK fitting at the top of the source housing 8 6 8 Cleaning the Ionization Source Capillary Plugging of the capillary either in the ESI or APCI probe causes the pressure o...

Page 215: ...for your system 8 6 9 Replacement of Ion Source Housing 1 Place the ion source housing on top of the base plate and line up with the rear electrical connection Push down until source chamber is seated evenly across the base plate 2 Finger tighten the two thumb screws and finger tighten the 28 PTFE tube fitting labeled as heated desolvation on the side of the housing 3 Follow the steps in Replacing...

Page 216: ...L 6 3 9 Press the Start Carrier Pump button Watch the pressure on the ribbon gauge Loosen the fitting at the source inlet If the pressure drops then the source capillary is plugged If there is still an error or the pressure remains high then the plug is between that point and the splitter valve or the valve itself Continue to loosen fittings going back the to the splitter valve until the error is ...

Page 217: ... is still incorrect replace the check valves The correct flow rate depends on the back pressure of the carrier solvent The flow will be 0 5 mL minute until the fluid interface reaches operating pressure then reduces the flow rate to 0 2 mL minute under typical operating conditions for the fluid interface The operating mode can be determined by listening to the pump operate While running at 50 ml m...

Page 218: ... to Instruction Sheet 60 5232 475 CombiFlash Rf Injection Valve Replacement 8 8 Electrical Troubleshooting If your instrument stops working and the touch panel display is off check the line cord connection If the line cord is connected properly check the fuses in the power input module located on the system s rear panel These are time delay fuses T type and rated according to the mains input power...

Page 219: ...C during standby The PurIon vacuum level is too low to operate Please verify that the roughing pump is on and operating correctly Pirani Pressure s1 mbar where s1 is the vacuum reading The Pirani pressure must be below 5 5E 3 mbar before the PurIon turbo pump will operate If trying to place the PurIon in operate without turning on the roughing pump this message will appear This error generally occ...

Page 220: ...echnician Error 309 The PurIon has reported that the ion source high voltage cable is not properly plugged into its socket This is the cable with the round connector and is to the right and behind the ion source This generally occurs upon changing or cleaning probes A plug has occurred in the PurIon fluid lines The separation can be continued without PurIon detection or continued if the plug is co...

Page 221: ...The fluid interface pressure is too low Error 325 This could be due to lack of carrier fluid loss of pump prime or leakage Table 8 3 General Troubleshooting Error Symptom Solution No signal on any mass or very weak signal Verify nitrogen pressure Nitrogen is required to nebulize the sample Check carrier solvent level refill carrier solvent and re prime the carrier solvent pump Carrier solvent is n...

Page 222: ...ings on the solvent interface Sample masses observedbutweak or masses other than the analyte observed Check polarity to see if the sample ionizes under the opposite polarity Try another ionization settings IONIZATION SETTINGS 6 3 10 Compound fragments use fragment mass or try another ionization setting Compound forms adducts Compound fails to ionize using the selected probe Some compounds ionize b...

Page 223: ...CombiFlash Rf User Manual 8 24 ...

Page 224: ...PO Box 82531 Lincoln NE 68501 2531 USA Attention Harold Hostetter The products listed below are eligible to bear the CSA Mark shown with adjacent indicators C and US for Canada and US or with adjacent indicator US for US only or without either indicator for Canada only Issued by PRODUCTS CLASS 8721 05 CLASS 8721 85 0 1 23 4 56 78 9 3 APPLICABLE REQUIREMENTS 5 3 3 6 0 9 3 3 6 9 ...

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Page 226: ... Level 2 4kV contact discharge Level 3 8kV air discharge A A EN61000 4 3 2010 Radiated RF Immunity 80 MHz to 2 7GHz 80 AM at 1kHz Level 1 10V m A EN61000 4 4 2010 Electrical Fast Transient on Mains and I O Level 2 2kV on ac lines A EN61000 4 5 2005 Surge on AC Lines 2kV common mode 1kV differential mode A EN61000 4 6 2008 Conducted RF on AC Mains and I O 150 kHz to 80 MHz 3V rms 80 modulated A EN6...

Page 227: ......

Page 228: ...tory Use Standard Description Severity Applied Performance Criteria EN61000 4 2 Electrostatic Discharge Level 2 4kV contact discharge Level 3 8kV air discharge A EN61000 4 3 Radiated RF Immunity 80 Mhz to 2 7Ghz 80 AM at 1kHz Level 2 3V m A EN61000 4 4 Electrical Fast Transient Level 2 1kV on AC lines A EN61000 4 5 Surge on AC Lines Level 2 2kV common mode Level 2 1KV differential mode A EN61000 4...

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Page 230: ...arge A EN61000 4 3 2006 A1 2007 A2 2010 Radiated RF Immunity 80 mHz to 2 7gHz 80 AM at 1 kHz Level 2 3V m A EN61000 4 4 2004 A1 2010 Electrical Fast Transient EFT on Mains and I O Level 2 1kV on AC lines A EN61000 4 5 2005 Surge on AC Lines Level 2 1kV Line Common Mode Level 2 0 5kV Differential Mode A EN61000 4 6 2008 Conducted RF Immunity on Mains and I O 150 kHz to 80 mHz Level 1 1V rms 80 Modu...

Page 231: ......

Page 232: ...kas Padhye Ph D Vice President and General Manager 4700 Superior Street Lincoln Nebraska 68504 Phone 402 464 0231 FAX 402 464 0318 This information is considered accurate and reliable as of the date appearing above and is presented in good faith Because use conditions and applicable laws may differ from one location to another and may change with time recipient is responsible for determining wheth...

Page 233: ......

Page 234: ... 摞 ST 㪖屓䤓棟摞尐㻑ⅴₚᇭ O Represent the concentration of the hazardous substance in this component s any homogeneous pieces is lower than the ST standard limitation X 嫷䯉年㦘㹡㦘䓸德咂年捷ↅ䤓㩟德㧟㠨䤓摞怔 ST 㪖屓䤓棟摞尐㻑ᇭ 㷳㫈㗽棔 ₙ嫷㓢 X 䤓㔏㦾扪嫛扪㷴広㢝ᇭ X Represent the concentration of the hazardous substance in this component s at least one homogeneous piece is higher than the ST standard limitation Manufacturer may give...

Page 235: ......

Page 236: ...ld under the Teledyne Isco trademark or for which any other warranty is specifically stated Damage to CombiFlash instruments resulting from the failure of a non RediSep column may cause the need for repairs that incur billable service activities The customer is responsible for these charges This warranty is expressly in lieu of all other warranties and obligations and Teledyne Isco specifically di...

Page 237: ......

Page 238: ...archive 4 archive how to 27 auto reports tools menu command 8 B backup 4 backup how to 27 basic method settings main window 14 batch run settings Rf 4x systems 26 button fast forward 15 next tube 15 pause 14 play 14 rewind 15 stop 15 bypass solid load cartridge 12 bypass solid load cartridge how to 55 C capacity tube 38 characters illegal 18 collecting peaks 21 collection ...

Page 239: ...ntrol manual 61 D default method description of 2 editing 53 defining a gradient overview 54 real time 54 delete files 4 delete files how to 27 delete gradient point 20 detection wavelength 14 double advance tube 48 drift tube temperature ELSD 24 E edit method menu 7 edit method window 49 editing default column programs 8 default method 53 gradient real time editing 54 method settings 46 ...

Page 240: ...s 3 file search 27 flash drive 4 flash drive save to 27 flow rate setting 18 foreign language 40 fraction collector specify rack 38 full scale percentage 22 full scale percentage edit method window details 50 G gradient defining 54 linear or step method 40 plot area 12 plot area batch 26 real time editing 54 table 20 gradient optimizer 25 H help contacting Teledyne Isco 3 menu command 10 hysteresi...

Page 241: ... 40 M main window 11 manual control how to 61 menu command 8 window 34 marks tube change 61 menu edit method 7 file 3 help 10 tools 8 method editor advanced method settings 17 method file description 2 editing 46 main window settings 14 scaling 5 mode peak collection 48 monitor peak detection how to 50 monitoring peak detection 23 monitoring solvent levels 36 ...

Page 242: ... menu command 9 pause button 14 peak collection mode described 48 edit method window 21 peak detection settings 49 slope 49 slope based 22 threshold edit method window 22 peak width 49 PeakTrak help 3 task examples 42 PeakTrak window 11 main region 2 menu bar window element 1 menus 3 play button described 43 main window 14 previous rack button 60 priming pump ...

Page 243: ...settings 2 RediSep Rf columns equilibration volumes 47 size edit method window 18 size main window 13 resetting column programs 8 rewind button 15 rows gradient 20 run control buttons 14 files 3 viewing 58 run length setting main window 20 S sample names main window 14 saving a file 3 scaling method files 5 search files 27 sensitivity peak detection edit method window 22 setting ...

Page 244: ...solvent management module inlet solvent assignment 36 solvent level monitoring controls 36 spray chamber temperature ELSD 24 starting a run 43 step gradient method 40 stop button 15 T threshold peak detection 22 threshold peak detection edit method window details 50 time windows 18 time windows setting 48 tools menu 8 tube advance 48 change marks 61 rack 38 volume 38 U USB flash drive 4 USB flash ...

Page 245: ...t 37 viewing a run 58 volume equilibrating RediSep columns 47 tube 38 W wavelength detection 14 monitoring 23 monitoring how to 50 width peak 22 window configuration 36 gradient optimizer 25 main 11 manual control 34 ...

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