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Thermo Scientific Dionex UltiMate 3000 Series, Operating Instructions Manual

The Thermo Scientific Dionex UltiMate 3000 Series is a sophisticated laboratory instrument designed for precise analyses. To ensure efficient operation, it is crucial to have the Operating Instructions Manual readily available. You can easily download this essential manual for free from our website, manualshive.com.

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UltiMate 3000 Series: 

NCS-3500RS and NCP-3200RS 

 

Page 

242

 

Operating Instructions

 

11.2  Optional Accessories 

Accessories 

Description 

Part No. 

Column Switching 

Valve 

2-position, 6-port switching valve 

2-position, 10-port switching valve 

6041.0004 

6041.0001 

Signal cable 

6-pin mini-DIN cable for connection to the Digital I/O port of 

the pump 

6000.1004 

Mixer kit (mixer 

volume: 8 µL) for 

capillaryLC 

To reduce the ripple for capillaryLC applications, connect the 

mixer capillary to the flow meter outlet and, by using the union 

from the mixer kit, connect the free end of the capillary to the 

other components of the HPCL system. 

6041.7895 

Upgrade kit for 

ProFlow flow meter 

Includes all required accessories for modification of a module 

with a ProFlow flow meter. 

Note:

 The ProFlow flow meter must be ordered separately. 

6041.3003 

Application kits for UltiMate 3000 RSLCnano systems 

The modules of UltiMate 3000RSLCnano system can be arranged in different 

configurations for various applications. All parts required for the system setups (columns, 

capillaries, fittings, etc.) are included in the related RSLCnano application kits.  
For information about how to arrange and set up an RSLCnano System, refer to the 

"UltiMate 30000 RSLCnano - Standard Applications" system manual. The manual is 

shipped with the NCS-3500RS and NCP-3200RS.

 

 

 

Direct Injection Nano LC Kit 

6720.0300 

 

Direct Injection Capillary LC Kit 

6720.0305 

 

Preconcentration Nano LC Kit 

6720.0310 

 

Preconcentration Capillary LC Kit 

6720.0315 

 

Preconcentration Monolithic LC Kit 

6720.0320 

 

2D Salt Plugs Kit 

6720.0325 

 

Automated off line SCX-RP Peptides Kit 

6720.0330 

 

Automated offline RP-RP Peptides Kit 

6720.0340 

 

Tandem Nano LC Kit 

6720.0335 

SRD-3x00 Solvent Racks

 

 

SRD-3200 

Solvent Rack with analytical 2-channel vacuum degasser 

5035.9250 

SRD-3400 

Solvent Rack with analytical 4-channel vacuum degasser 

5035.9245 

SRD-3600 

Solvent Rack with analytical 6-channel vacuum degasser 

5035.9230 

SR-3000 

Solvent Rack (without vacuum degasser) 

5035.9200 

Summary of Contents for Dionex UltiMate 3000 Series

Page 1: ...c Dionex UltiMate 3000 Series Nano Cap System NCS 3500RS Nano Cap Pump NCP 3200RS Operating Instructions Original Operating Instructions Revision 2 0 Date January 2016 2016 Thermo Fisher Scientific Inc Doc No 4820 4101 ...

Page 2: ...UltiMate 3000 Series NCS 3500RS and NCP 3200RS Operating Instructions ...

Page 3: ...4 Front Panel Elements 22 2 5 Rear Panel 24 2 5 1 Power Switch 25 2 5 2 Fuse Cartridge 25 2 5 3 USB Port 25 2 5 4 Digital I O 25 2 5 5 Solvent Rack 25 2 6 Interior Components 26 2 7 Fluid Connections 27 2 8 Pump Module 29 2 8 1 Rear Seal Wash System 29 2 8 2 Flow Meter 30 2 8 3 Leak Sensor 32 2 8 4 Purge Valve 32 2 8 5 Inline Filter Loading Pump 33 2 9 Column Compartment 34 2 9 1 Gas and Humidity ...

Page 4: ...ting the Solvent Reservoirs 63 4 4 Connecting Drain Tubing 65 4 5 Pump Module 67 4 5 1 Setting Up the Rear Seal Wash System 67 4 5 2 Flow Meter Settings 69 4 5 3 Purging the Pumps 72 4 6 Column Compartment 78 4 6 1 Installing a Column Switching Valve 78 4 6 2 Installing a Separation Column 80 4 6 3 Installing a Trap Column 82 4 6 4 Connecting the Components to the Column Switching Valve 82 4 7 Equ...

Page 5: ...a and Equilibration Time 136 5 7 4 Using the Digital Inputs and Outputs Digital I O 137 5 7 5 Operational Qualification and Performance Qualification 137 5 8 Recommendations for Optimally Running Systems Best Practice 138 5 9 Shutting Down the Module 140 5 10 Maintenance and Maintenance and Calibration Intervals 142 5 10 1 General Information 142 5 10 2 Maintenance Intervals 143 5 10 3 Calibration...

Page 6: ...ng the Purge Screw Loading Pump 210 7 11 Testing the Loading Pump for Leakage 211 7 12 Column Switching Valve 213 7 12 1 Replacing the Column Switching Valve 213 7 12 2 Replacing the Valve Stator and Rotor Seal 214 7 13 Replacing the Main Power Fuses 216 7 14 Updating the Firmware 217 8 Module Specific Information 219 8 1 NC Pump 220 8 1 1 Interior Components Detailed View 220 8 1 2 Flow Path 221 ...

Page 7: ...ference Information 247 12 1 Chemical Resistance of PEEK 247 12 2 Solvent Miscibility 250 12 3 Properties of Common Solvents 251 12 4 Safety Information about Flammable Solvents 252 13 Appendix 255 13 1 Digital I O Pin Assignment 255 13 2 Solvent Rack Pin Assignment 256 14 Index 257 ...

Page 8: ...UltiMate 3000 Series NCS 3500RS and NCP 3200RS Page vi Operating Instructions ...

Page 9: ...icro pump referred to as loading pump If a description refers to the NC pump and the loading pump the term the pump module or the pump is used If some detail applies to only one pump the pump is identified by name The NCP 3200RS is a binary high pressure gradient pump HPG referred to as NC pump This pump corresponds to the NC pump in the NCS 3500RS Therefore the descriptions for the pump module an...

Page 10: ... be liable for incidental or consequential damages in connection with or arising from the use of this document We appreciate your help in eliminating any errors that may appear in this document The information contained in this document is subject to change without notice All rights reserved including those for photomechanical reproduction and storage on electronic media No part of this publicatio...

Page 11: ...l opérateur et ou protéger le module contre tout dommage Label according to the Measures for Administration of the Pollution Control of Electronic Information Products China RoHS guideline Étiquette Measures for Administration of the Pollution Control of Electronic Information Products China RoHS WEEE Waste Electrical and Electronic Equipment label For more information see the WEEE Information sec...

Page 12: ...ir compte de l information jointe peut conduire à de faux résultat ou endommager l instrument Warning Indicates that failure to take note of the accompanying information may result in personal injury Avertissement Indique que ne pas tenir compte de l information jointe peut entraîner des blessures corporelles ...

Page 13: ...guidelines of Good Laboratory Practice GLP An eyewash facility and a sink should be close to the device If any substance splashes on the eyes or skin wash the affected area and seek medical attention Hazardous substances Many organic solvents mobile phases and samples are harmful to health Be sure that you know the toxic and infectious properties of all substances that you are using You may not kn...

Page 14: ...tem some components are made of PEEK This polymer has superb chemical resistance to most organic solvents However it tends to swell when in contact with trichlormethane CHCl3 dimethyl sulfoxide DMSO or tetrahydrofuran THF In addition it is attacked by concentrated acids such as sulfuric acid and nitric acid or a mixture of hexane ethyl acetate and methanol In both cases capillaries may start leaki...

Page 15: ... from buffer to organic solution rinse the pump thoroughly with deionized water When switching to another solvent ensure that the new solvent is miscible with the one contained in the pump If the solvents are not miscible the pump can be damaged for example by flocculation Use only standard solvents MS grade and buffers that are compatible with all parts in the module that may be exposed to solven...

Page 16: ...ted to the module to prevent evaporation in the flow cell Always use the frits recommended by Thermo Fisher Scientific This is to prevent particulate matters from entering the HPLC system Using other frits may considerably affect the system performance If a leak occurs stop the pump flow turn off the module and remedy the situation Before interrupting operation for several days or more or when pre...

Page 17: ...sécurité des substances que vous utilisez Veuillez respecter des directives des Bonnes Pratiques de Laboratoire BPL Une installation permettant de se laver les yeux ainsi qu un lavabo doivent se trouver à proximité du système Si une substance quelle qu elle soit entre en contact avec vos yeux ou votre peau rincez abondamment la zone affectée à l eau puis Substances dangereuses De nombreux solvants...

Page 18: ...lvants au réservoir de déchets Capillaires électriquement conducteur devrait être mis à la terre Inflammation spontanée des solvants N utilisez aucun solvants avec une température d auto inflammabilité inférieure à 150 C Si une fuite se produit ces solvants peuvent s auto enflammer au contact d une surface chaude Capillaires connecteur capillaires connexions ouvertes Des capillaires en particulier...

Page 19: ...tre démontés uniquement par le personnel de service de Thermo Fisher Scientific Remplacez les câbles de communication défectueux Remplacez les cordons d alimentation électrique défectueux Utilisez uniquement les cordons d alimentation électrique spécifique à l instrument Remplacez toujours les fusibles grillés par des fusibles de rechange autorisés par Thermo Fisher Scientific Utilisez seulement d...

Page 20: ...le NCS seul Ne placez aucun objet lourd sur la porte ouverte du panneau avant Ceci pourrait endommager la porte Afin d éviter que le calibrage de pression de la pompe de chargement ne soit pas entravé mettez en marche la pompe seulement quand la pompe est sans pression Toujours ouvrez la vis de purge avant mettre la pompe en marche Ne faites jamais fonctionner la pompe à sec Il peut en résulter de...

Page 21: ...nt Avant d interrompre le fonctionnement pendant plusieurs jours ou plus observez les précautions figurant en page 140 N utilisez pas l instrument de manière autre que celles décrites dans ce manuel Conservez ce manuel á proximité de l instrument pour pouvoir le consulter facilement Veuillez noter Veuillez noter aussi les recommandations pour la bonne pratique en section 5 8 page 138 ...

Page 22: ...d spare parts recommended by Thermo Fisher Scientific page 239 and within its technical specifications page 235 If there is any question regarding appropriate usage contact Thermo Fisher Scientific before proceeding Thermo Fisher Scientific cannot be held liable for any damage material or otherwise resulting from inappropriate or improper use of the instrument Warning If the device is used in a ma...

Page 23: ...to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment This equipment generates uses and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause harmful interference to radio communications Operation of this equipment in a residential area is likely to cause harmful interf...

Page 24: ...UltiMate 3000 Series NCS 3500RS and NCP 3200RS Page 16 Operating Instructions ...

Page 25: ...roFlow flow meter and thus is the appropriate choice for ultra high performance LC UHPLC applications Key features of the pump module The NC pump includes two highly precise constant pressure pumps that are controlled by closed control loops and that enable continuous operation without the need of refill cycles The flow meter controls the partial flows of the two channels The integrated control pr...

Page 26: ...ax 75 C At an ambient temperature of 25 C an increase in temperature from 35 C to 65 C is typically realized in 12 minutes Temperature control allows keeping the column temperature constant within the specified range The maximum deviation is 0 1 C An electronic column identification module allows GLP compliant documentation of the column type and all important column parameters page 34 Various mon...

Page 27: ...pump with Classic flow meter for capillary LC loading pump and column compartment Basic version without column switching valves The NCP 3200RS nanoLC ProFlow can be fitted with a Classic flow meter for capillary LC applications page 202 Micro LC The NCS 3500RS nanoLC ProFlow NCS 3500RS capillaryLC and NCP 3200RS nanoLC ProFlow can be fitted with a Classic flow meter for micro LC applications page ...

Page 28: ...gasser 5035 9245 SRD 3600 Solvent Rack with analytical 6 channel vacuum degasser 5035 9230 SR 3000 Solvent Rack without degasser 5035 9200 In an UltiMate 3000 RSLCnano system a SRD 3400 Solvent Rack with analytical 4 channel vacuum degasser should be used together with the NCS 3500RS Tip If the UltiMate 3000 system includes an UltiMate 3000 series autosampler you should degas also the wash solutio...

Page 29: ...ndividual components of the module see section 8 For the Find information about the On page NC pump Interior components detailed view Liquid flow path Operating principle 220 221 222 Loading pump Interior components detailed view Liquid flow path Operating principle 226 227 228 Column compartment Interior components detailed view Operating principle 229 230 ...

Page 30: ...andby button for at least one second If you switch a module to which a SRD 3x00 Solvent Rack is connected to the Standby mode the Solvent Rack too will be set to Standby mode 2 Lever Moves the valve actuators or if already installed the column switching valves toward the front page 78 3 Display Shows information about the pump upper display and about the column compartment lower display Status scr...

Page 31: ...n Chromeleon Status Status LED pump module The LED is green when the pump is ready for operation The LED is red when an error has been detected for example a leak Status LED column compartment The LED is green when the column compartment has reached the target temperature The LED is orange when the column compartment has not yet reached the target temperature or when the door is open The LED is re...

Page 32: ...O ports page 25 for communication with external devices for example a mass spectrometer 5 Solvent Rack port for connection of a SRD 3x00 Solvent Rack page 25 6 USB hub 3 USB ports for USB 2 0 or 1 1 Depending on the UltiMate 3000 system configuration for connection of one UltiMate 3000 system module each or for connection of one USB hub each page 25 7 USB port USB 2 0 or 1 1 for connecting the mod...

Page 33: ...to Dionex instruments Thermo Fisher Scientific cannot guarantee correct functioning if third party instruments are connected Important Thermo Fisher Scientific recommande d utiliser les ports USB uniquement pour les raccordements aux instruments Dionex Thermo Fisher Scientific ne peut garantir le bon fonctionnement si les instruments d autres fabricants sont raccordés For information about how to ...

Page 34: ...escription 1 NCS 3500RS only Column compartment here with one column switching valve detailed view page 229 2 Pump module with No Description 3 NC pump detailed view page 220 4 Detector of rear seal wash system page 29 5 Peristaltic pump of the seal wash system page 29 6 Flow meter of the NC pump page 30 7 NCS 3500RS only Loading pump detailed view page 226 6 3 2 1 7 5 4 ...

Page 35: ...e in the pump module Column Compartment Unlock the front panel door as shown in the picture The door tilts downward To close the column chamber tilt the front panel upward The door locks automatically Fig 5 Unlocking the front panel door Important The open front panel doors of the pump and column compartment are not designed to carry weight Therefore you should not place any objects on the open do...

Page 36: ...S Page 28 Operating Instructions When connecting the capillaries and routing them to other system modules observe the general information in section 4 2 page 57 For more information about the liquid flow paths in the module see section 8 page 219 ...

Page 37: ... consists of a peristaltic pump a detector and a reservoir containing seal wash solution The wash solution passes the individual components as shown in Fig 6 Fig 6 Rear seal wash system here in the NCS 3500RS The arrows indicated the flow path of the wash solution through the pump For information about how to set up the rear seal wash system see page 67 For more information about how to operate th...

Page 38: ...n with thermal flow sensors Note Operation of the module with a ProFlow flow meter requires a suitable firmware and Chromeleon version For details contact Thermo Fisher Scientific sales organization 6041 7850 Classic flow meters with flow selector for Capillary LC 0 5 10 µL min 6041 7902A Micro LC 5 50 µL min 6041 7903A Flow selectors for Classic flow meters Flow selector for capillary LC 0 5 10 µ...

Page 39: ...ilt in inline filter From right pump head to flow meter 3 Flow meter outlet pump outlet From flow meter to autosampler Tip Operation of the module with a ProFlow flow meter requires a suitable firmware and Chromeleon version Classic Flow Meter Flow Connections Fig 8 Classic flow meter No Description No Description 1 Flow meter inlet from left pump head 4 Capillary from right pump head to flow mete...

Page 40: ... page 124 2 8 4 Purge Valve NC pump Both pump heads solvent channels of the NC pump have their own purge valve with purge screw and purge outlet The purge screw and purge outlet are located in the flow meter above the pump head to which they belong Fig 9 Purge valves of the NC pump here Classic flow meter Loading pump The loading pump has a purge unit that comprises the purge valve with purge scre...

Page 41: ...nstructions Page 33 2 8 5 Inline Filter Loading Pump The loading pump has an inline filter that is located below the pump head The filter volume is 10 µL The filter frit is a titanium frit with a porosity of 2 µm Fig 11 Inline filter loading pump Inline filter ...

Page 42: ...te the source for the leakage page 178 2 9 2 Column Switching Valves The column compartment can be equipped with one or two column switching valves page 19 and thus provides highest flexibility for all applications that required different columns at similar temperatures The switching valves are installed in the column chamber where they are brought to the preferred temperature together with the co...

Page 43: ... Tip All software details in this manual refer to Chromeleon 6 80 If you want to operate the module from Chromeleon 7 availability with Chromeleon 7 1 and later refer to the following documents for information about how to perform the related processes in Chromeleon 7 all documents are included in the Chromeleon 7 shipment Chromeleon 7 Help provides extensive information and comprehensive referenc...

Page 44: ...o detect liquid leaks page 32 Leak sensors in the column compartment to detect excessive gas and or humidity page 34 Electronic column identification system to provide a GLP compliant overview of the column status page 34 When an error is detected the Status LED on the related front panel door is red a beep sounds and a message appears on the pump display page 147 When the module is operated from ...

Page 45: ... the surface is resistant to solvents Avoid locations with extreme changes in temperature Also avoid locations with extreme direct sunlight and high humidity Allow sufficient clearance behind and to the sides of the module for ventilation and do not place any objects between the module and the module located below it in the system stack 3 2 Unpacking All electrical and mechanical components of the...

Page 46: ...bulky for one person alone to lift or move safely Important Afin d empêcher l instrument de tomber saisissez la par les côtés Ne soulevez l instrumente à l aide du matériau d emballage ou par les portes des panneaux avants Le NCS 3500RS et lourd et encombrant Par conséquent vous ne devriez pas soulever l instrument seul 4 Remove the foam spacers and then remove the polythene packaging 5 Tilt the f...

Page 47: ...nterconnect them on the rear panel Fig 13 The arrangement of the system modules depends on the application For information about how to arrange and set up an RSLCnano System refer to the UltiMate 30000 RSLCnano Standard Applications system manual The system manual is shipped with the module Fig 12 Module arrangement for an UltiMate 3000 RSLCnano system example Autosampler WPS 3000TPL RS Solvent Ra...

Page 48: ... computer with only one connection For systems with a VWD 3400RS use only the hub on the NCS 3500RS or NCP 3200RS respectively For systems with a DAD 3000RS or MWD 3000RS detector you can use only the hub on the detector Apart from the Solvent Rack all modules of the UltiMate 3000 RSLCnano system can be connected also separately to the Chromeleon computer by using the USB port on the rear panel of...

Page 49: ...o the Chromeleon computer by using the USB ports on the rear panel Fig 2 page 24 Select one of the following alternatives Connect the module directly to the USB port on the Chromeleon computer Connect the module to the computer by using an external USB hub However this may be the source for communication problems depending on the quality of the hub Tip The USB standard limits the USB cable length ...

Page 50: ...in D Sub connector on the rear panel of the Solvent Rack The appropriate connection cable is included in the accessories kit of the Solvent Rack 3 4 5 Connecting Devices Mass Spectrometers to the Digital I O Port To connect a device for example a mass spectrometer to a digital I O port on the rear panel of the module use a 6 pin mini DIN signal cable part no 6000 1004 The cable is available from T...

Page 51: ...he computer is a network computer 3 Open the Chromeleon Server Monitor program by double clicking the Chromeleon Server Monitor icon on the Windows taskbar If the Server Monitor icon is not on the taskbar click Start on the taskbar point to Programs or All Programs depending on the operating system point to Chromeleon and then click Server Monitor 4 Click Start to start the server 5 Click Close to...

Page 52: ...nect to Windows Update to search for software select No not this time b Accept the default option Install the software automatically and click Next c Click Finish when the wizard reports that the software for the module has been installed If Windows fails to detect the module and a message box asks for a USB configuration file cmwdmusb inf this indicates that you connected the module to the comput...

Page 53: ...erver name to display the items underneath 4 Select the timebase to which the module will be assigned or create a new timebase on the Edit menu click Add Timebase 5 Open the Add device to timebase dialog box To do so click Add Device on the Edit menu or right click the timebase and click Add Device on the menu 6 On the Manufacturers list click Dionex HPLC UltiMate 3000 and on the Devices list clic...

Page 54: ...ettings on the configuration pages For additional information about a page click Help General Page Display general information about the module Fig 14 General page Device Type Indicates the device model Enable Virtual Mode This check box should be cleared because Chromeleon only simulates the functions of the module when the virtual mode is active If the Virtual Mode is enabled the Module Address ...

Page 55: ...lays the name used to identify the pump module in the installation environment and in the Chromeleon client Under PumpModule the following commands and properties are displayed for example in the Commands dialog box page 89 General properties and commands related to the entire pump module such as the commands and properties for the seal wash system leak detection or the degasser in a SRD 3x00 Solv...

Page 56: ...pecific groups of properties and commands are listed in the Commands dialog box for the related pump There you can set for example the flow rate and the partial flows change the upper and lower pressure limits and start a purge cycle To control the pump with the existing control panels accept the default name If you enter different names you may have to re link the controls on the control panels a...

Page 57: ... specific limits on a control panel or in a program file Solvents Page The loading pump and the NC pump of the NCS 3500RS have separate Solvents pages Check and change the number of solvents delivered by the pump and the solvent names if necessary Number of Solvents Indicate how many solvents are delivered by the pump The pump type determines how many solvents can be delivered Pump Type Max Number...

Page 58: ...name you may have to re link the controls on the control panels and edit the name of the column compartment in the program files Temperature Channel default name ColumnOven_Temp The Use Channel check box is selected by default Accept this setting if you want to record the temperature of the column compartment as a separate channel page 131 The name specified in the Channel Name text box is used to...

Page 59: ...n the control panels and edit the column name in the program files The information about the column is continuously updated and can be reviewed at any time in Chromeleon page 129 Signals Page The Signals page lists all available signals Select a check box to enable the signal If a check box is cleared the signal will not be available in Chromeleon To change a signal name or the scaling factor over...

Page 60: ...is detected automatically and displayed on the Flowmeter page Flowmeter Type To be able to use a certain solvent with the NC pump consider the correct setting for the respective flow meter ProFlow flow meter With a ProFlow flow meter the flow meter must know the solvent type The solvent list shows the pre defined and user defined solvents for each pump block channel Classic flow meter With Classic...

Page 61: ...ings reopen the configuration pages 1 Start the Server Configuration program page 45 2 Right click the module in the timebase and click Properties on the menu 3 Change the settings as needed For a description of the pages see section 3 5 3 1 page 46 4 To save the configuration click Save Installation on the File menu and then close the Server Configuration program ...

Page 62: ...UltiMate 3000 Series NCS 3500RS and NCP 3200RS Page 54 Operating Instructions ...

Page 63: ...ect the 15 pin D Sub port on the rear of the Solvent Rack with the Solvent Rack port on the rear of the module page 25 2 If you want to connect a mass spectrometer to the module Connect the Digital I O port on the rear of the module with the appropriate port on the mass spectrometer page 42 3 Connect the solvent reservoirs page 62 4 Connect drain tubing page 65 Important If drain tubing is not con...

Page 64: ...f necessary page 125 8 Column Compartment a Install the valves if required page 78 b Install the separation columns page 80 c Install a trap column if required for your application page 82 d Establish the fluid connections between the columns and switching valves as required by your application For information about how to connect the capillaries to the valve see section 4 6 4 page 82 e Turn on te...

Page 65: ...utlet Tip Viper or nanoViper capillaries with torque toothing cannot be connected to the flow meter outlet When you connect capillaries make sure that the connectors are free from contaminants Even minute particles may cause damage to the system Different fitting systems are used in an UltiMate 3000 system Therefore install the capillaries and fittings only at the positions for which they are inte...

Page 66: ...is observed at the connection port remove the capillary clean the capillary ends carefully by using a cloth or tissue wetted with isopropanol and reinstall the capillary If the connection continues to leak install a new Viper capillary Viper fitting with knurled screw Loosen or tighten these Viper connections only by using the black knurled screw and only with your hand do not use tools If you obs...

Page 67: ...s If you observe leakage on the connection tighten a little further If leakage still exists clean the connection port with a cleaning swab part no 6040 0006 If this does not eliminate the problem replace the capillary and or fitting To avoid increased dead volume or damage to the system and leakage reuse fittings and ferrules only for the same capillary connection ...

Page 68: ... the pump module for example to secure the solvent lines to the interior front panel of the pump Fig 21 Clips in the pump module Column Compartment Capillaries to be routed to the outside on the sides of the column chamber have to be routed through the guides provided on the left and right of the column chamber Fig 22 Capillary guides here on the right of the column chamber Capillaries to be route...

Page 69: ... a 90 degree angle related to the door seal An improper seal may reduce the heating performance of the column compartment Clips to secure any capillaries routed from the top to the bottom of the column chamber are provided in the accessories kit of the NCS 3500RS Insert the capillary into the left or right side of the clip and attach the clip to the enclosure bottom Fig 23 Fig 23 Clip with capilla...

Page 70: ... degasser in the Solvent Rack The procedure how to prepare and install the liquid lines for the wash solution is similar to the steps for the solvent supply lines For more information see the Autosampler manual 4 3 1 General Notes When connecting the solvent reservoirs observe the following general precautions Before using the solvent reservoirs for the first time rinse them thoroughly by using hi...

Page 71: ...ss 4 3 2 Connecting the Solvent Reservoirs 4 3 2 1 NC Pump The solvent supply lines are connected to the NC pump at the factory Solvent lines for NC pumps with a ProFlow flow meter are equipped with shut off valves Connect the solvent supply lines directly to the solvent reservoirs 1 Feed the solvent supply line through the retaining guide which holds the tubing in place in the reservoir Then feed...

Page 72: ... can close the shut off valves instead 4 3 2 2 Loading Pump 1 Prepare the solvent reservoirs as described in section 4 3 2 1 page 63 2 The solvent supply lines are connected to the loading pump at the factory Connect the solvent supply lines from the reservoirs and from the pump to the degassing module of the Solvent Rack For information about how to connect the tubing to the degasser see the Solv...

Page 73: ...e lab bench direct the tubing over the edge of the lab bench and place the free end of the tubing into the waste container Installation Instructions of the UltiMate 3000 drain system b If the module is not the bottom module in the UltiMate 3000 system stack Install an elbow to the port connect drain tubing of suitable length and place the free end of the tubing into the waste container Rear port L...

Page 74: ... connection port Fig 28 and fill in MS grade water until the liquid exits the drain port at the bottom right of the module Fig 28 Filling water into the connection port 3 Verify that the liquid is discharged properly If it is not any modules that are located below this module in the UltiMate 3000 system stack may suffer severe damage from the liquid leaving the drain port 4 Reconnect the seal wash...

Page 75: ...elease the lever Fig 29 Peristaltic pump 2 Fill the seal wash reservoir 250 mL a reservoir is provided in the accessories kit of the NCS Observe the precautions for the composition of the seal wash solution on page 122 3 Connect the silicone tubing from the peristaltic pump with the seal wash reservoir If necessary prolong the tubing Silicone tubing is provided in the accessory kit of the module 4...

Page 76: ... pump to the right so that the liquid can easily pass the system c Reconnect the tubing to the detector Connect the tubing to the inner port Fig 30 page 67 The outer port has no function 7 Verify that the seal wash solution is discharged properly page 66 For information about how to operate the pump with rear seal washing and for details about what happens see section 5 5 7 page 122 ...

Page 77: ...re of water and acetonitrile 20 80 v v Classic flow meter With the viscosity values of the most common solvents for example water acetonitrile and methanol and mixtures such as mixtures of water and acetonitrile 50 50 v v or 20 80 v v If the solvent that you want to use is not available in the solvent list ProFlow flow meter or viscosity list Classic flow meters in Chromeleon refer to section 5 5 ...

Page 78: ...nd then select the preferred solvent from the list Tip If you are using a solvent with up to 2 additive it is sufficient to select the main solvent Solvent mixtures with higher percentages of a component require a solvent calibration Fig 31 Setting the solvent type ProFlow flow meter only If the solvent type that you are using is not yet available in the list perform a solvent calibration for the ...

Page 79: ... for the solvent to be added to the list in Chromeleon Type a viscosity value that has been established earlier as described in this manual directly in the input box Note that values entered here will not be added to the Chromeleon viscosity list This value will be used until you establish and save a new value or enter a different value in Chromeleon Note the following for the solvent viscosity se...

Page 80: ... solvents If the pump has not been purged sufficiently pressure pulsation a high noise level or pulsation during the operation of the pump may occur or the analysis may not be reproducible Due to the large liquid volumes in the NC pump and the low flow rates during operation it is especially important that the pump is purged sufficiently long Only then you can be sure that the previous solvent has...

Page 81: ...low the connection to be opened Empty the solvents lines If solvent shut off valves are installed on the solvent lines you can close the shut off valves instead 4 5 3 1 1 Purging the Pump Heads 1 Attach a syringe to the free end of the silicone tubing on the purge nozzle of the pump head left head right head or both that you want to purge Two syringes are provided in the accessories kit of the mod...

Page 82: ...servoirs you should purge the pump head to make sure that the fresh solvent is available throughout the system The purge time depends on the flow meter installed ProFlow flow meter Purge for about 5 minutes Classic flow meter Purge for about 10 minutes When changing solvents to a different type If you want to change solvents purge the pump head to make sure that the previous solvent is completely ...

Page 83: ...lves if they are not yet closed Turn the purge screw clockwise with your hand to the stop 2 Connect the nanoViper capillary 0 25 x 155 mm I D x L MP35N from the accessories kit of the module to the flow meter outlet The other end of the capillary must remain open 3 Purge the flow meter from Chromeleon or from the pump display To purge the flow meter from Chromeleon a In Chromeleon open the Command...

Page 84: ...further up on this page While the flow meter is being purged the pressure at the flow meter outlet is monitored internally However the column pressure reading does not reflect the actual column pressure As a result an overpressure condition can occur even thought the column pressure reading is still 0 bar In this case remove any components from the flow meter outlet that can cause a pressure build...

Page 85: ...le for all channels of the loading pump even if they are not used for the application until all air bubbles are gone To purge the pump from the pump display a On the pump display select the Control menu for the loading pump page 101 b Set the channel to be purged to 100 for example A Start the purge cycle To do so set Purge to On The pump is purged with the Purge Flow and Purge Time settings from ...

Page 86: ... carrying out any work in the column compartment wait for the column chamber to cool down To shorten the cool down time consider setting a lower temperature and opening the front panel door 2 A lever is provided on the enclosure bottom of the column compartment for pulling forward the valve actuators Turn the lever to right and pull it toward the front as far as it goes out Fig 35 Pulling the valv...

Page 87: ...e 106 On the pump display from the Control menu of the NC pump or loading pump page 101 Select the preferred menu and select Catch Left Valve Head or Catch Right Valve Head b The actuator starts turning slowly Push the valve onto the actuator while the actuator is moving The valve locks in place as soon as the actuator is in the correct position 5 In Chromeleon or on column compartment display che...

Page 88: ... shipped together with the column clips To protect the column attach one pad to the inside of each bottom part Fig 38 Attaching a pad inside the column clip 3 Do not touch any metal or plastic parts inside the column chamber while the temperature is higher than 50 C Before carrying out any work in the column compartment wait for the column chamber to cool down To shorten the cool down time conside...

Page 89: ...40 Attaching the column ID to the column 6 Press the column into the bottom part of the clip and reinstall the ring Fig 41 Installing a column in the clip 7 Connect the capillaries to the column and establish the fluid connections between the separation column and the column switching valve For information about how to connect the capillaries to the valve see page 80 When connecting the capillarie...

Page 90: ...l information about how to connect capillaries page 57 4 6 4 Connecting the Components to the Column Switching Valve 1 Do not touch any metal or plastic parts inside the column chamber while the temperature is higher than 50 C Before carrying out any work in the column compartment wait for the column chamber to cool down To shorten the cool down time consider setting a lower temperature and openin...

Page 91: ...plication 3 Set the detector wavelengths and turn on the lamps 4 Monitor the pump pressure Verify that the reading is correct for the application and is stable Loading pump only The compression value should remain stable under 100 The compression value is displayed for example on the Diagnostics menu for the loading pump page 102 5 Monitor the detector signal and verify that the baseline signal is...

Page 92: ...UltiMate 3000 Series NCS 3500RS and NCP 3200RS Page 84 Operating Instructions ...

Page 93: ... the module appears on the front panel displays device type serial number and firmware version The module runs a series of internal tests During these self diagnostics all of the main components are checked When the self test was successful the status screens appear on the front panel displays page 85 If an error is detected the module or the component for which the error is detected is not ready ...

Page 94: ...n the Properties dialog for the module in the Chromeleon Server Configuration program page 48 Flow on or Flow off or Purge Flow on appears when the pump delivers with the specified flow rate Flow off appears when the pump is not delivering Purge appears when a purge cycle is running Flow rate When the pump is pumping the display always shows the flow rate that the pump is actually delivering When ...

Page 95: ...1 1 2 C Setpoint 40 0 C Left Right Fig 43 Status screen example Under The following information appears Compartment Current column temperature in C Setpoint Target temperature for temperature control in C The temperature value is flashing until the selected temperature is reached Off is displayed when temperature control is disabled Switching Valves Flow path in the column switching valves if inst...

Page 96: ...y are not yet running page 43 2 Start the Chromeleon client by clicking the Chromeleon icon on the desktop If the Chromeleon icon is not on the desktop click Start on the taskbar point to Programs or All Programs depending on the operating system point to Chromeleon and then click Chromeleon 3 Connect the Chromeleon client program to the timebase in which the module is installed For details about ...

Page 97: ...se tab For more information about the Timebase dialog click Help Tip The Control menu is visible only when a control panel is already open 3 Press the F8 key or select Command on the Control menu 4 Show the parameters and commands for the components of the module They appear under the names specified for the components in the Properties dialog for the module page 47 a Click the plus sign next to P...

Page 98: ... Connect command Tip The Connect command is listed under PumpModule When you perform the Connect command the column compartment is automatically connected too For a list of the commands and parameters that are supported for the module see the Chromeleon Help In addition to the commands and parameters for this module the Commands dialog box provides also access to all commands and parameters availa...

Page 99: ...r the module Fig 46 Control panel here for the NCS 3500RS 3 Verify that the module is connected in Chromeleon the LED next to the Connect button is green If the module is not yet connected click Connect The control panel provides access to the operating parameters and commands required for routine operation of the module Additional functions are available in the Commands dialog box To open the Com...

Page 100: ...p To create a program with the Program Wizard 1 Open the Program Wizard On the File menu select New and then select Program File 2 The wizard guides you through program creation On each wizard page accept or change the settings as appropriate For additional information about a page click Help 3 After you finish the wizard Chromeleon automatically creates the corresponding program 4 To start the pr...

Page 101: ...the entire program listing the control commands in chronological order For more information see the Chromeleon Help 3 To start the program follow the steps in the next section To start a program Program for sample analysis 1 Create a sample list sequence A sequence must include the program and a method for evaluating the sample data for example for peak identification area determination and amount...

Page 102: ...g 48 Showing the function keys The function keys replace the information in the bottom line of the status screen If no key is selected the bottom line of the status screen is restored after about 5 seconds When the module is connected in Chromeleon the function keys except Menu are not available The following function keys are available for the pump Function Key Description Menu Opens the Main men...

Page 103: ... Purge on the Control menu page 101 The following function keys are available for the column compartment Function Key Description Menu Opens the Main menu page 105 Temp Opens the Temperature menu Under Temperature Control you can turn temperature control on and off Under Temperature you can set the target temperature Valve Opens the Valves menu Under Left Valve Position and Right Valve Position yo...

Page 104: ... 104 The general layout and structure is identical for all menus section 5 4 2 1 5 4 2 1 General Menu Layout and Structure In general the menu layout is as follows Control 1 4 1 Flow 2 Flow rate 3 A 4 B Select Back 1 2 3 Fig 49 Menu layout here Control menu for the pump No Description 1 Reports the menu name and the number of items on the menu list 2 The menu items appear on a list and are numbere...

Page 105: ... for example the settings for the leak sensor or Proceed to the next figure in a number Any decimal point is skipped Confirm the selection and activate the input field if applicable If an item is read only the Select key will not be available Select Perform the selected command Execute Return to the previous menu level Back Toggle between two operating states for example between On and Off Toggle ...

Page 106: ...1 through 5 4 2 2 5 page 100 and following pages Section 5 4 2 1 provides information about the general menu layout and function keys on the navigation bar page 96 1 Control 2 Preferences 3 Diagnostics Main 1 Self Test 2 Model 3 Firmware Version 4 Bootloader Version 1 Flow 2 Flow Rate 3 A 4 B 4 Configuration 1 Display Soft Keys 2 Leak Sensor Mode 3 Pressure Unit 5 Max Pressure 6 Min Pressure 7 Pur...

Page 107: ...sion 1 Flow 2 Flow Rate 3 A 4 B 4 Configuration 1 Display Soft Keys 2 Leak Sensor Mode 3 Pressure Unit 5 C 6 Max Pressure 7 Min Pressure 8 Purge 9 Change Pump Pistons 10 Catch Right Valve Head 11 Catch Left Valve Head 1 Degasser 2 Purge Time 3 Purge Flow 4 Flow Acceleration 5 Flow Deceleration 5 Firmware Version 7 Serial Number 4 Reset to Factory Defaults Fig 51 Loading pump menus ...

Page 108: ...ration page 101 Preferences On the Preferences menu you can make the basic settings for the related pump page 102 Diagnostics The Diagnostics menu provides information for diagnostic purposes read only In addition you can perform a self test for the pump module page 102 Configuration The Configuration menu provides information about the configuration of the pump module and allows you to make the r...

Page 109: ...r flow meter The component is purged for the Purge Time specified on the Preferences menu page 102 Loading pump The loading pump is purged with the Purge Flow and Purge Time settings specified on the Preferences menu page 102 For more information about how to purge the pumps see section 4 5 3 page 72 Purge Open the Pump Maintenance dialog for piston and piston seal replacement From this dialog you...

Page 110: ... flow rate deceleration For details see page 119 Flow Deceleration 5 4 2 2 4 Diagnostics Menu The Diagnostics menu provides information for diagnostic purposes read only In addition you can perform a self test for the pump module To Select Perform a self test Tips Before performing the command open the purge valves to reduce any pressure and to avoid that pressure builds up The self test is perfor...

Page 111: ... sets the screen contrast The input is in percent Key sound sets whether a beep sounds when you select a function key Key autorepeat sets whether the keystroke is automatically repeated when you remain on the key for a longer period for example to change a value quickly Display Soft Keys Turn leak detection off if necessary and on again Disabled turns leak detection off Enabled turns leak detectio...

Page 112: ... 5 4 2 3 4 page 105 and following pages Section 5 4 2 1 provides information about the general menu layout and function keys on the navigation bar page 96 Main 3 Configuration 1 Display Soft Keys 2 Left Valve Config 3 Right Valve Config 1 Control 1 Temperature Control 3 Left Valve Position 2 Information 1 Heating Workload 2 Temperature 4 Right Valve Position 4 Gas Leak Mode 5 Humidity Leak Mode 6 ...

Page 113: ...ettings or change the settings page 106 5 4 2 3 2 Control Menu From the Control menu you can turn temperature control on and off and set the target temperature In addition you can specify the switching position of the valves To Select Turn temperature control on or off Temperature Control Set the target temperature Temperature Set the switching position for the left valve liquid flow path through ...

Page 114: ...eak detection is performed and how you are alerted in case of an alarm Select the sensor and set the sensitivity Low Standard or High turns leak detection on and sets the sensitivity with which the sensors respond to excessive gas or humidity When a sensor is activated a message appears on the pump display and a beep alerts you when set under Leak Alarm Mode Off turns leak detection off Gas Leak M...

Page 115: ...y NC pump 114 Setting the flow rate flow acceleration and flow deceleration 119 Setting the pressure limits 120 Recording the pump pressure 121 Rear seal washing 121 Purging the pumps 124 Detecting liquid leaks in the pump module 124 Adjusting the screen brightness or contrast 125 Operating the degasser of a SRD 3x00 Solvent Rack 125 Section 5 6 page 127 provides information that should be conside...

Page 116: ... the operating instructions for the modules Make sure to use special highly pure solvents They are usually labeled accordingly by the vendor Mind the special properties of the solvents such as viscosity boiling point UV absorption UV VIS detector refractive index refractive index detector and dissolved gas degasser pH range 2 10 Do not operate the module with solvents that at the same time have ve...

Page 117: ...e of PEEK see the table in section 12 1 page 247 Before switching from buffer to organic solution rinse the pump thoroughly with deionized water When switching to another solvent ensure that the new solvent is miscible with the one contained in the pump Otherwise the pump can be damaged for example by flocculation When replacing solvents make sure that the solvents are miscible Mix immiscible solv...

Page 118: ...sure the current flow rates and the pump speeds are controlled so that the flow rates match the set values Both partial flows are mixed in a microfluidic Y piece no 6 at the flow meter outlet Fig 53 Functional blocks of the NC pump with ProFlow flow meter No Element 1a 1b Flow controlled pump left A and right B 2a 2b Dual piston pump left right 3a 3b Filter unit left right 4a 4b Primary pressure t...

Page 119: ...u use 100 water in solvent channel A and acetonitrile water 80 20 in solvent channel B at a flow rate of 1500 nL min check the table entry for acetonitrile water 80 20 above a maximum column pressure of 890 bar is possible with the pump The Ready Check checks if the selected flow rate can be delivered reliably at the selected maximum column pressure If this is not possible a message appears If the...

Page 120: ...e picture illustrates how the pump operates with a Classic flow meter For more information about the operating principle of the NC pump see page 222 Fig 54 Functional blocks of the NC pump with Classic flow meter No Element 1a 1b Pressure controlled pump left A and right B 2a 2b Dual piston pump left right 3a 3b Filter unit left right 4a 4b Primary pressure transducer left right 5a 5b Flow restric...

Page 121: ...MPa Solvent B is the lower viscosity solvent and thus can be ignored This means min nL MPa MPa MPa min nL Flow max 875 20 65 100 100 100 500 The Ready Check checks whether the selected flow rate can be reliably delivered with the selected maximum column pressure page 120 A message appears if this is not possible If the upper limit for the column pressure is set to a value that is considerably high...

Page 122: ...roFlow flow meter for this solvent type and add the solvent type to the list in Chromeleon Note the following For solvent calibration the solvent shut off valves need to be installed During solvent calibration select the respective pump block channel left right of the flow meter for which you want to calibrate the solvent Solvent types are only available in the block channel for which they are cal...

Page 123: ...re 4 Complete the solvent calibration as instructed in the wizard Make sure that you update the solvent or viscosity list in the device configuration by selecting the Update button on the Flowmeter page 5 5 3 2 Performing a Solvent Viscosity Measurement Classic Flow Meter Relevant only for NC pump with Classic flow meters If the viscosity for the solvent that you are using is not yet known page 69...

Page 124: ...nter a different value in Chromeleon for example in the Commands dialog box or on the control panel for the module Limited or Failed The viscosity measurement has been passed only with limitations or failed Follow the instructions provided by the wizard and repeat the procedure 4 Write down the viscosity value if you want to use it later again see further down or if you want to add it to the visco...

Page 125: ...t not start with a digit The name must be unique Avoid entries with different names but identical viscosities values Combine these entries instead Fig 55 Fig 55 Entering the viscosity Chromeleon always uses the entry for a specific viscosity that appears first on the viscosity list Fig 56 Therefore if more than one entry exists for a specific viscosity the Chromeleon report may not show the name o...

Page 126: ...alog box for the NC pump under A_Viscosity and B_Viscosity for example Solvent1_81_4 Fig 56 Showing the viscosity Observe the following The viscosity list applies to all module instances that are installed on the same Chromeleon server Changes and new entries appear only for the module for which you have made them on the Viscosities page in the Server Configuration program To make the new entries ...

Page 127: ...w acceleration and flow deceleration in Chromeleon 1 In Chromeleon open the Commands dialog box for the pump page 89 2 Select Flow and enter the flow rate in the Nominal box The allowed flow rate range is indicated in the Properties dialog for the module page 48 In the Properties dialog box you can change the upper and lower limit for the flow rate within the allowed range 3 Under MaximumFlowRampU...

Page 128: ...per pressure limit Helps to protect the column from too high a pressure The application and column type determine the setting When setting the upper pressure limit for the NC pump observe the information in section 5 5 2 page 110 To set the pressure limits in Chromeleon A Pressure range The range within which the pressure limits can be set and the pressure unit are specified in the in the Properti...

Page 129: ...n provide helpful information to identify and eliminate the source for the problem Therefore always record the signals of your module The signal default name Records the following signal NC_Pump_Pressure Column pressure of the NC pump Selected by default LoadingPump_Pressure Pressure of the loading pump Selected by default ProFlow flow meter only If a ProFlow flow meter is installed make sure that...

Page 130: ... the precautions for the composition of the seal wash solution page 122 There will be a warning when the reservoir is empty Rear seal wash system has run out of wash solution Nevertheless check the liquid level in the seal wash reservoir at regular intervals Regularly check the volume in the waste container for the seal wash solution Empty the waste container as needed 5 5 7 2 Choosing the Seal Wa...

Page 131: ...stem has run out of wash solution If the rear seal liquid is not discharged properly to the waste the following message may appear The rear seal leak sensor detects drops constantly Take the following remedial action Check the seal wash reservoir level Replace the peristaltic tubing Verify that the liquid can pass the tubing properly Replace the tubing if required Clean the detector electrodes pag...

Page 132: ...t panel door is red A message appears in Chromeleon and on the pump display The Leak property in Chromeleon is set to Leak A beep alerts you The pump stops the flow if the leak sensor reports a leak for at least 3 minutes When the leak sensor reports a leak Locate the source for the leak eliminate the cause and dry the leak sensor page 177 You can disable the alarm temporarily To do so open the Co...

Page 133: ...powered up the SRD is powered from the module The degasser is ready for operation To turn the degasser on and off from the pump display Select the Preferences menu page 102 and set Degasser to On or Off To turn the degasser on and off from Chromeleon 1 In the Server Configuration program open the Properties dialog for the module page 53 2 On the Pumps page verify that Degasser Control is set to Ex...

Page 134: ...mmends always leaving the degasser on while the pump is on Turning off the module to which the SRD is connected also turns off the SRD The same applies to Standby mode Also observe the information about the solvent compatibility of the degasser page 108 In addition observe the general information about how to operate the degasser Solvent Rack manual ...

Page 135: ...rmation about special Chromeleon functions see section 5 7 page 132 5 6 1 Turning On Temperature Control You can turn temperature control on and off and set the target temperature in Chromeleon and on the column compartment display Tip The column compartment has no active cooling system and thus the temperature in the compartment cannot be reduced below a temperature resulting from the ambient tem...

Page 136: ...u change the temperature setting under Nominal Chromeleon sets TempCtrl automatically to On To turn on temperature control on the display column compartment 1 Show the function keys and select Temp or select the Control menu 2 Select Temperature and enter the temperature Temperature control becomes active and Temperature Control is automatically set to On Set Temperature Control to Off if you do n...

Page 137: ...formation will be available for the column in Chromeleon 4 The information on the column ID chip card see further down is continuously updated and can be reviewed at any time in Chromeleon for example in the Commands dialog box for the column oven under Column_A B C or D as long as the column and chip card are installed in the column compartment Column Properties The chip card provides the followi...

Page 138: ...isplay To adjust the sensitivity from Chromeleon 1 In Chromeleon open the Commands dialog box for the column compartment 2 Select GasLeakSensor or select HumidityLeakSensor and set the sensor sensitivity Select Low Standard or High When the sensor is activated The Status LED on the front panel door is red A message appears in Chromeleon and on the pump display Select Off to deactivate leak detecti...

Page 139: ... the temperature signal channel can provide helpful information to identify and eliminate the problem 5 6 5 Adjusting the Screen Brightness or Contrast You can adjust the screen brightness or screen contrast to your requirements from Chromeleon or on the column compartment display To do so select one of the following alternatives In Chromeleon open the Commands dialog box for the column compartmen...

Page 140: ...nd for monitoring and recording service and re qualification information Open the Commands dialog box page 89 and enter the limits for the predictive performance parameters The predictive performance counters and commands for the components of the module are grouped in Wellness sections for example PumpModule_Wellness LoadingPump_Wellness and ColumnOven_Wellness To keep the predictive performance ...

Page 141: ...lp Control Panel On the control panel for the module click Wellness Qualification and Service to see the related predictive performance commands and parameters on separate panels On these panels you can enter the limits and reset the counters In addition wellness bars provide visual indicators of qualification and service periods The color coding of the wellness bars provides information about the...

Page 142: ...are available for the devices in the current timebase Select a test A wizard guides you through the test For more information about a test see the Chromeleon Help Pump To check the Run the Loading pump Degasser vacuum in a SRD 3x00 Solvent Rack that is operated from the pump Degasser Vacuum Test Loading pump Loading pump system especially the fitting connections for leakage General Leak Test Loadi...

Page 143: ...mp and the flow rate accuracy and or determine the viscosity for the solvents used with the NC pump page 114 Viscosity Measurement NC pump Only NC pump with ProFlow flow meter installed The zero balance of the flow sensors and set them to zero if required See section 6 6 1 page 172 Recommendation If you want to test the NC pump for tightness by running the Detailed Leak Test run the Zero Balance T...

Page 144: ...ple Temperature set point 45 C ReadyTempDelta 1 C The column compartment is ready for operation when the current temperature is between 44 C and 46 C If the current temperature is outside this range the column compartment enters the NotReady state If ReadyTempDelta is set to None Chromeleon does not check whether the current temperature deviates from the temperature set point Equilibration Time In...

Page 145: ...fy that The device you want to control is connected to the digital I O port on the rear panel of the module page 42 and that the appropriate signal cable 6 pin Mini DIN part no 6000 1004 is used for the connection The relay outputs and digital inputs you want to use are selected in the Properties dialog for the module page 52 When these conditions are fulfilled the relay outputs and digital inputs...

Page 146: ...ou can check and correct the offset of the pressure transducers if required To do so run the Pressure Transducer Test page 172 If a ProFlow flow meter is installed you can check and adjust the zero balance of the flow sensors if required To do so run the Zero Balance Test page 172 A drift or shift in retention times can also have other reasons that are not connected to the sensors For example you ...

Page 147: ...lvents are always fresh and that they have been properly prepared After preparation degas the solvents by ultrasonication to remove the excess air that could have introduced from the mixing 6 Before running any calibration routines perform a purge cycle page 72 to ensure that the pump is properly primed 7 Flow meter settings For Classic flow meters Run a viscosity measurement to determine and set ...

Page 148: ...e pump with methanol or a similar alcohol such as isopropanol or ethanol If the solvents in the pump are not miscible with water use an appropriate intermediate solvent If a buffer is used as a part of the mobile phase flush the system with several volumes of methanol water 50 50 before it is shut down This is to prevent salt buildup inside the unit If pump operation is interrupted for more than 5...

Page 149: ...ning Chromeleon you can set the module and HPLC system into the standby mode or automate system shutdown Standby Program A standby program sets the HPLC system into standby mode The main program steps are At the end of the program the program automatically reduces the flow The program reduces temperature of all temperature controlled modules in the system From the standby mode you can reactivate t...

Page 150: ...remain open When internal maintenance is complete the purge cycle starts automatically If no purge cycle is initiated after another 6 weeks a message appears in the Chromeleon Audit Trail reminding you to start a purge cycle NC pump When the fluid components of the NC pump are filled with liquid and the solvent reservoirs are located above the pump outlet during pump operation the hydrostatic pres...

Page 151: ...he pump for leakage at least once a month page 186 Check the filter frits in the solvent supply line filters for permeability Replace the filter frits in regular intervals This is especially important with aqueous solvents Aqueous solvents may contaminate the filters with algae and other microorganisms that deposit on the filter frits Therefore use fresh the solvents at regular intervals Rinse the...

Page 152: ...ave a small drift When the drift is large enough a small shift in retention times can be observed This does not mean that the instrument is broken However mind the following for the pressure transducers and thermal flow sensors If a Classic flow meter is installed you should check and correct the offset of the pressure transducers if required To do so run the Pressure Transducer Test page 172 If a...

Page 153: ...on of the module a message appears on the pump display For information about the possible causes along with recommended courses of action see page 147 and the following pages If the module is operated by Chromeleon a message is also displayed in the Chromeleon Audit Trail Tip For information about operating problems that might occur during the operation of an UltiMate 3000 system see Operating Pro...

Page 154: ...ch of the past three strokes If the compression value is lower than 100 for several strokes afterward the message Compression back to normal will appear in the Audit Trail For more information about the compression values see section 6 7 page 174 During pump maintenance The pistons are in the appropriate position for piston seal replacement The LED flashes red The pistons are not in the appropriat...

Page 155: ... message relates may appear in front of the message text In addition to the messages listed in the table other messages may appear If you cannot eliminate the problem note the exact wording of the message Contact Thermo Fisher Scientific Service for Dionex HPLC Products Message Remedial Action x autozero flow failed Drift was too high where x specifies if left or right flow sensor Wait until the m...

Page 156: ...s properly connected to the P Sys connector for the loading pump on the interior front panel Open and close the purge valve if necessary to reduce the pressure Can t start pump while alarm is on An alarm has occurred for example a leak alarm You can restart the pump flow only after having acknowledged the alarm for example by performing the AlarmOff command in Chromeleon Cannot deliver desired flo...

Page 157: ... of the degasser in the Solvent Rack was activated The vacuum level is insufficient The Solvent Rack may not be connected properly to the module Verify that the Solvent Rack is properly connected to the module Turn the Solvent Rack off and on again by pressing the standby button on the front panel The degassing module may be defective and should be replaced by your Service representative Flow cali...

Page 158: ...ansducer Test page 172 2 From Chromeleon perform the CalibrateWP command for the pump head Flow meter temperature out of range The temperature of the flow is outside the allowed range The flow meter may be defective Replace the flow meter page 202 Flow meter data version mismatch The firmware installed in the module does not support the full functionality of the flow meter You should update the fi...

Page 159: ...re or Implausible left primary pressure or Implausible right primary pressure The pressure values established during the self test are not plausible Turn the module off and on again by pressing the power switch on the rear of the module Contact Service if the message appears again Depending on the flow meter that is installed proceed as follows ProFlow flow meter Perform the Zero Balance Test page...

Page 160: ...bration values established during pump operation for the left and or right pump head of the NC pump are not plausible The cable for the related pressure transducer may not be connected properly Verify that the cable properly connected Perform the following sequence of actions 1 ProFlow flow meter Perform the Zero Balance Test page 172 Classic flow meter Run the Pressure Transducer Test page 172 2 ...

Page 161: ...ears again Left working piston drive sensor remains dark Drive initialization failed for the left working piston of the NC pump Turn the module off and on again by pressing the power switch on the rear of the module Contact Service if the message appears again Motor current too large The motor current is too high when the loading pump is running The flow path before the transducer for the system p...

Page 162: ...re If the message appears during the internal maintenance procedure for the loading pump page 142 perform an additional purge cycle for the loading pump page 76 Pressure fallen below lower limit The solvent reservoirs are empty Fill the reservoirs and purge the pump page 72 There are air bubbles in solvent supply line Check the filter frits and purge the system page 72 The system is leaking Find a...

Page 163: ... valve moving to position timeout The right valve did not reach the specified position within a certain time There may be no valve installed or the valve is not configured properly Check and change the valve type in Chromeleon or on the oven display page 50 or page 106 if required and switch the valve again Contact Service if the message appears again Right valve position error The right valve did...

Page 164: ...ston seals page 194 The pressure exceeded the absolute limit The pressure has exceeded the absolute pressure limit This message appears when pressure builds up extremely fast NC pump Each pressure transducer of the NC pump can cause this message First verify that the pressure transducer cables are properly connected on the flow meter Disconnect and reconnect the cable Then make sure that the press...

Page 165: ...ng connectors as necessary The peristaltic tubing may be blocked or draws air Replace the tubing if necessary page 180 Inspect the rear seal wash tubing for indications of leakage page 179 Replace the seal wash tubing and the tubing connectors as necessary Verify that the lever of the peristaltic pump Fig 29 page 67 is not blocked Inspect the electrodes of the seal wash detector for indications of...

Page 166: ...may be contaminated Rinse or replace the column The autosampler may be blocked Find and eliminate the source for the blockage If the flow path is not blocked Check the permeability of the filter frit in the inline filter Replace the filter frit if necessary page 209 The switching valve in the column compartment may not have switched properly In this case an additional message will appear for the v...

Page 167: ...ay be interrupted Check the USB connection The power supply to the module may be interrupted Check the power supply connection of the module Error issuing control request to NCS 3500 USB 1610103 The USB connection between the module and the Chromeleon server may be interrupted Check the USB connection Check the power supply connection of the module Remove the module specified in the message from t...

Page 168: ...Probable Cause Remedial Action The capillary connections are leaking Check all fluid connections for indications of leakage Find and eliminate the source for the leak Tighten leaking connections If the leakage continues replace the capillaries Capillaries with Viper fitting connections Perform this sequence of actions Remove the capillary carefully clean the capillary ends by using a cloth or tiss...

Page 169: ...est continues to fail information about possible causes and suggested remedial actions are provided also on the last page of the wizard guiding you through the test Follow these instructions and repeat the test The purge screw may be open Close the purge screw The piston seals may be worn out Perform a detailed leak test page 134 Replace the piston seals page 194 The capillary between pump head an...

Page 170: ...aking Replace the piston seals page 194 Backpressure may have fluctuated due to problems with the restrictor The restrictor may be blocked Replace the restrictor The pressure was outside specification The pressure was outside the upper and lower pressure limits Repeat the test with changed flow settings The compression value was over the limit There are air bubbles in the pump Purge the pump page ...

Page 171: ...1 The fuses blow Replace the fuses page 212 Replacement fuse blows immediately Contact Service An error occurred in the electronic system Contact Service The module does not work correctly when controlled by Chromeleon There is no connection between the module and the Chromeleon computer Check the USB cable and connection to the computer The USB port on the computer is not ready for operation Chec...

Page 172: ...ching valve if installed or the injection valve is blocked Check and replace the valve if necessary The column is contaminated or blocked Rinse or replace the column The loading pump has very high backpressure The filter frit on the high pressure side of the loading pump is dirty Replace the filter frit page 209 High baseline drift The column is contaminated Clean or replace the column The system ...

Page 173: ... Calibrate the pressure transducers page 172 The solvent settings are incorrect Check and correct the settings for the solvents in Chromeleon Solvents were pre mixed and not used for a longer period of time Purge the pump page 72 Pre mixed solvents are too old Use fresh eluent Use fresh and appropriate solvents MS grade Purge the pump page 72 High noise level non periodic baseline fluctuation The ...

Page 174: ...nections Replace the capillaries Consider using Viper capillaries Peak Broadening increased dead time The inner diameter of the capillary to the detector is too large Use a capillary with an appropriate inner diameter The filter frits on the solvent supply lines are clogged Check the filter for permeability Replace the filter frit if necessary page 62 With the NC pump the message Cannot regulate f...

Page 175: ...ce the flow rate from the loading pump and or reduce the loading time Reproducible ghost peaks in the chromatogram The degassing channels are contaminated Rinse the degassing channels Solvent Rack manual The eluents are degraded dirty or of poor purity quality Use fresh solvent Use fresh and appropriate solvents MS grade Contamination occurs somewhere in the system Flush the system with an appropr...

Page 176: ...ge 72 The gradient is irreproducible The pressure transducer offset may not be correct Check the offset and calibrate the pressure transducers if required page 172 The sample is unstable and decomposes Use new sample or change the conditions Cool the sample in the autosampler if possible Baseline fluctuations See the remedial actions provided in the related baseline sections further up in this tab...

Page 177: ...erform a wash cycle Non degassed wash solution is used Degas the wash solution Autosampler manual After a maintenance procedure replacement of pump head piston or piston seal the pistons are not in the appropriate position for normal operation Remove and reinstall the pistons pages 188 and 190 NC pump with Classic flow meter Flow fluctuation flow is too low poor gradients The flow selector is clog...

Page 178: ...low rate UV signal drift during the gradient In applications with TFA the TFA concentration is incorrect If the signal drifts upward solvent B contains too much TFA and vice versa Increase or reduce the TFA concentration as needed After switching from the loading pump flow to the nano flow there is a drop in the UV signal and the signal does not return to the initial level fast enough The trap col...

Page 179: ... are placed in such a manner that ambient air can enter the column chamber Verify that the capillaries are routed correctly through the guides on the sides of the column chamber and or rest flat on the edge of the enclosure section 4 2 2 page 60 Temperature control is turned off The following information appears on the status screen Setpoint Off Check and change the temperature control setting pag...

Page 180: ... Pressure Transducer Test to verify that the pressure transducer offset is still correct If it is not calibrate the pressure transducers Before you begin Observe the Tips and Information for performing the test further down in the section 1 In Chromeleon open a control panel and connect to the timebase in which the module is installed page 89 2 On the Control menu select Diagnostics and then selec...

Page 181: ...ong as the retention times are stable and in the expected range you should not interrupt pump operation by recalibrating the pressure transducers You should check also the offset of the pressure transducers Before you test the NC pump for leakage by running the diagnostics functions from Chromeleon Observe the recommended order of tests page 134 If you observe a shift in peaks or if the gradients ...

Page 182: ...compression value should be lower than 100 and remain stable If the value is close to 100 the required precompression may not be reached and pulsation may occur The table shows guides values for some solvents Solvent Compression Acetonitrile 70 10 Methanol 75 10 Water 50 10 with 100 of degassed solvent delivered at 40 MPa pump purged and stable for some time The values are linear to the pressure I...

Page 183: ...ur la manipulation correcte des composés et des recommandations pour les situations de risque spécifiques veuillez consulter la fiche de données de sécurité des substances que vous utilisez Veuillez respecter des directives des Bonnes Pratiques de Laboratoire BPL Before starting maintenance or service procedures observe the following precautions For all service and repair procedures observe all pr...

Page 184: ...iginal packaging and observe the packing instructions when shipping the module Shipping the module in anything other than the original packaging voids the warranty If the original shipping container is not available appropriate shipping containers and packing material can be ordered from Thermo Fisher Scientific sales organization for Dionex HPLC products The packing instructions are included in t...

Page 185: ...r Fig 60 Drying the leak sensor 4 Allow the sensor to adjust to the ambient temperature for a few minutes The red sensor LED should now be dark The yellow LED may be dark or illuminated this LED does not indicate errors 5 If no errors are reported you can resume operation 6 Loading pump only Test the loading pump for leakage after you have carried out maintenance or repair work on the fluid connec...

Page 186: ...1 Find and eliminate the leak wearing appropriate protective clothing 2 Beeping stops for the current alarm when you open the front panel door 3 Ventilate the interior of the column chamber thoroughly only then close the front panel door 4 If the sensor is not activated again after the door has been closed you can resume operation Tip The Status LED for the column compartment remains red as long a...

Page 187: ... tubing Press the lever of the peristaltic pump to the right so that the liquid can easily pass the system 3 Press the lever of the peristaltic pump firmly onto the tubing and then press liquid into the seal wash system from the syringe 4 Inspect the tubing and connections of the seal wash system for indications of leakage Tighten or replace leaking connections as necessary 5 Connect the seal wash...

Page 188: ...ect the other end of the peristaltic tubing from the seal wash tubing clear tubing 5 Locate the PharMed tubing white tubing in the Tubing Kit for the Rear Seal Wash System and cut the tubing to the required length 6 Connect the replacement tubing to the connection port on the pump head and to the tubing from the seal wash reservoir Push the PharMed tubing onto the connector as far as it goes on a ...

Page 189: ...tector from the drain port of the seal wash system by pulling the detector upward The detector cable remains connected in the pump 3 Clean the electrodes with distilled water and wait until they are dry The electrodes in the detector are critical for proper operation Therefore be careful not to bend or otherwise damage them during cleaning Fig 63 Detector of the seal wash system 4 Reinstall the de...

Page 190: ...nd outlet check valves Observe the information about the different fitting connections on page 57 To remove the capillary on the outlet valve nut consider disconnecting the other end of the capillary on the rear lower connection port first to facilitate the procedure 5 Loosen the check valve nuts by using an open end wrench size 13 and remove them from the pump head 6 Hold the nuts over your hand ...

Page 191: ... the inlet valve take care to avoid cross threading If the valve leaks you may tighten the fitting a little more Outlet check valve Tighten the Viper fitting connection Observe the information about the different fitting connections on page 57 10 To prevent contaminants from entering the HPLC system thoroughly rinse the pump page 72 11 Loading pump only Test the pump for leakage page 211 Tighten l...

Page 192: ... Operating Instructions 7 6 Pistons and Piston Seals Fig 65 Pump head pistons and piston seals Depending on the pump version the representation of a part may be different from the real part However the position of the parts is the same for all pump versions ...

Page 193: ...p head bushing N a 6 Support ring for the main piston seal 6040 0012 7 Main piston seal reversed phase 6266 0305 2 seals 8 Seal ring rear seal wash system Included in 6040 2208 9 Pump head N a 10 Valve cartridge same as no 12 6041 2301 11 Valve nut inlet check valve Included in 6042 7007 12 Valve cartridge same as no 10 6041 2301 13 Valve nut outlet check valve Included in 6042 7007 14 Tubing conn...

Page 194: ...test for the NC pump make sure that the following conditions are fulfilled The loading pump is not delivering The pressure of the loading pump is down to zero 5 Purge the flow meter page 75 6 To evaluate possible leakage observe the air liquid level in the silicone tube Finish the observation before a new seal wash cycle starts If the level remains unchanged the piston seals seal tightly Proceed w...

Page 195: ...C pump is down to zero 5 Set the flow rate Arrange the system in such a way that approximately 30 MPa of backpressure is produced 6 To evaluate possible leakage observe the air liquid level in the silicone tube Finish the observation before a new seal wash cycle starts If the level remains unchanged the piston seals seal tightly Proceed with the next step A rising level indicates leakage from one ...

Page 196: ...In Chromeleon open the Commands dialog box for the NC pump or the loading pump and perform the UndockPistons command For the NC pump the command appears under NC_Pump_Wellness_LeftBlock and NC_Pump_WellnessRightBlock for the loading pump the command appears under LoadingPump_Wellness_RightBlock Wait until the PistonPositionStatus property reports Undocked before you continue with the next steps 5 ...

Page 197: ... if you want to replace only the main piston seals Loading pump The pistons are removed from the pump together with the pump head Hold down the plate of the rear seal wash system on the pump head and remove the pistons from the head If the plate of the rear seal wash system remains in the pump when you remove the pump head set the pump head tool to the plate Fig 67 The pump head tool is provided i...

Page 198: ...lace the spacing tool on the plate of the rear seal wash system and push both pistons downward as far as possible The distance is correct when both pistons touch the spacing tool Remove the tool Fig 68 Establishing the distance 2 Place the pump head back into the pump and tighten the pump head screw with the hexagon wrench size 6 from the accessories kit of the module recommended torque 10 Nm If b...

Page 199: ...lling the pump head you removed If messages relating to the working pressure appear on the pump display for example Implausible right working head pressure or Implausible left working head pressure verify that the cable of the related pressure transducer is properly connected When installing a replacement pump head Messages relating to the working pressure of the pump appear on the pump display Ig...

Page 200: ... are closed e In Chromeleon perform the CalibrateWP command for the replacement pump head The command appears in the Commands dialog box for the NC pump under NC_Pump_Wellness_LeftBlock and or NC_Pump_Wellness_RightBlock Execution of the command takes about 30 seconds A message appears only if an error has occurred Note A primary pressure of 90 MPa builds up during calibration If you have replaced...

Page 201: ...ts Operational before you continue with the next steps 6 Flush the pump head with seal wash solution step 1 on page 186 7 To prevent contaminants from entering the HPLC system thoroughly rinse the pump page 72 8 Test the pump for leakage page 211 Tighten leaking connections 9 Update the service information in Chromeleon page 132 ...

Page 202: ...ead consists of 1 Removing the pump head and pistons page 188 2 Disassembling the pump head and removing the pistons seals page 195 3 Cleaning the pistons page 196 4 Reassembling the pump head page 197 5 Recommended Replacing the piston seals in the plate of the rear seal wash system page 199 6 Installing the pistons and pump head page 190 7 After replacing the piston seals observe the recommendat...

Page 203: ...st remove the support ring Tap the pump head on a surface to make the support ring drop out If this does not remove the support ring push the seal insertion tool into the pump head and remove the tool The support ring is removed together with the tool Tip Do not use the seal removal tool for the support ring because the ring can be removed from the tool only with difficulties 5 Remove the piston s...

Page 204: ...be clean consider performing the fingernail test in addition Hold the piston and carefully move your fingernail over the surface After performing this test you have to clean the piston again The piston is clean when the surface is completely smooth no inconsistent or rough areas Fig 71 Fingernail test 1 Carefully rinse the piston preferably with isopropanol and then rub it several times with a dry...

Page 205: ...ort ring is not a wear part and thus you need not replace the support ring when you replace the piston seal However before reinstalling the support ring you should clean the support ring from the inside and outside by using isopropanol a cleaning swab part no 6040 0006 and a lint free cloth or tissue 2 Pipette a few drops of isopropanol onto the edge in the pump head on which the piston seal will ...

Page 206: ...side faces the plate of the rear seal wash system Fig 74 Orientation of the rear seal wash body 7 If required place the plate of the rear seal wash system onto the pump head as shown in the picture The channels in the plate are facing you Fig 75 Plate of the rear seal wash system installed 8 Install the pistons and pump head page 190 9 After replacing the piston seals observe the recommendations o...

Page 207: ... wash system 3 Set the seal insertion tool to the side of the seal on the low pressure side of the plate as shown in the picture and push the seal out of the plate Fig 76 Removing the seal from the plate of the seal wash system 4 Insert and push the replacement seal into the plate high pressure side with your hand To prevent contamination put on a pair of gloves Fig 77 Inserting the piston seal in...

Page 208: ...rder 1 Zero Balance Test 2 Detailed Leak Test For Classic flow meter Run the following diagnostic tests in the given order 1 Pressure Transducer Test 2 Detailed Leak Test 3 Viscosity Measurement If Viscosity Measurement fails the new seals may not yet seal sufficiently tight Purge the flow meter for another 30 to 60 minutes page 75 and repeat the test Loading pump Never run the pump dry Damage to ...

Page 209: ...ncreased leakage rate after several hours of operation If leakage is observed with new piston seals operate the pump for at least 2 hours at 35 MPa to run in the seals It does not help if you tighten the pump head screw more Tip If the piston seals do not yet seal sufficiently tight try the following Have the pump build up high pressure page 211 and hold the pressure for some minutes ...

Page 210: ...n à la terre appropriée 1 Turn off the module by pressing the power switch on the rear of the module 2 Unplug the pressure transducer cables 3 Disconnect the capillaries connected to the flow meter inlets and outlet Fig 78 Flow meter here Classic flow meter 4 Loosen the two screws that attach the flow meter and pull the flow meter out toward the front 5 With Classic flow meters only Replace the fl...

Page 211: ...under NC_Pump_Wellness_LeftBlock and or NC_Pump_Wellness_RightBlock 13 Required only if a ProFlow flow meter was installed Purge the flow meter again page 75 14 Recommended for Classic flow meters Repeat the Pressure Transducer Test when the module has been operated with the new flow meter for about one day Allow a warm up period of 24 hours for the new flow meter to achieve optimum reproducibilit...

Page 212: ...onnectors are free from contaminants and close the open ends with the black caps Particles may clog the flow selector 1 Remove the flow meter page 202 2 First remove the screw that attaches the flow selector Fig 79 Flow selector 3 Afterward remove the capillaries marked a through d in the picture in any order 4 Remove the flow selector 5 Install the replacement flow selector in the reverse order T...

Page 213: ...r inlets on the ProFlow flow meter accommodate a built in inline filter each If a filter frit is clogged replace the filter frit Description Part No Filter frits for inline filter 2 frits porosity 2 µm 6268 0036 To replace the filter frit in an inline filter on the inlet of the ProFlow flow meter follow these steps 1 Stop the pump flow 2 On the ProFlow flow meter disconnect the capillary from the ...

Page 214: ...lvent line Follow these steps 1 Stop the pump flow and wait until the pressure is down to zero 2 Unscrew the cap of the solvent reservoir and remove the solvent line together with the cap from the reservoir 3 Purge the pump until the solvent line is empty 4 Proceed as required If the solvent line is to be replaced a Disconnect the solvent line from the reservoir cap b Connect the new solvent line ...

Page 215: ...off valve 3 Disconnect the elbow tubing from the pump head and empty the line into waste 4 Unscrew the cap of the solvent reservoir and remove the solvent line together with the cap from the reservoir 5 Empty the solvent line to the reservoir into waste 6 Disconnect the shut off valve with the elbow tubing from the solvent line to the reservoir 7 Connect the solvent line between pump head inlet an...

Page 216: ... filter frit in the inline filter also from Chromeleon by running the Mixer Frit Test page 134 7 9 2 Replacing the Inline Filter Description Part No Inline filter volume 10 µL with filter frit porosity 2 µm 6042 5014 Capillary from purge unit to inline filter Included in 6041 3001 1 Disconnect the capillaries on the filter inlet and outlet and remove the inline filter from the pump Fig 81 Inline f...

Page 217: ...nline filter as described in section 7 9 2 2 Open the inline filter and remove the filter frit 3 Pipette a drop of solvent into the frit holder and insert the replacement frit Close the filter housing The solvent keeps the frit in the holder during closing 4 Install the inline filter as described in section 7 9 2 5 Test the loading pump for leakage page 211 6 After you have replaced the filter fri...

Page 218: ...e unit Turn the screw counterclockwise all the way and then pull it straight off the purge unit 4 Before installing the replacement purge screw clean the hole in the purge unit with a cleaning swab part no 6040 0006 5 Hold the replacement purge screw carefully You should not hold the screw by the seal end to avoid scratching the seals These scratches will prevent proper seal and allow leakage Fig ...

Page 219: ...ow as soon as the pressure builds up typically between 20 and 30 MPa 5 Have the pump deliver some µL min until a pressure of 45 MPa has built up 6 When this pressure has been built up and when the pump delivers a flow of 1 µL min the pressure should increase or remain constant at least If it does not this indicates possible leakage 7 Find and eliminate the cause for the leak and then perform the t...

Page 220: ...ation time monitor the pressure drop d Tighten the connection a little more tight The pressure will suddenly increase a little e Monitor if the pressure drops at the same rate as before If the pressure drops significantly slower the connection was leaking 8 In Chromeleon reset the upper pressure limit to the value used before the leak test Tip If leakage from a pump head is observed check also the...

Page 221: ...004 2 position 10 port switching valve 6041 0001 Both valves are suitable for pressures 86 MPa 12500 psi 1 Do not touch any metal or plastic parts inside the column chamber while the temperature is higher than 50 C Before carrying out any work in the column compartment wait for the column chamber to cool down To shorten the cool down time consider setting a lower temperature and opening the front ...

Page 222: ...nt panel door 2 Pull the column switching valves toward the front To do so turn the lever for the actuators to the right and pull it toward the front as far as it goes out Fig 35 page 78 3 Grasp the valve for which you want to replace the stator and or rotor seal and pull firmly to remove the valve from the actuator 4 Remove the stator screws by using a hexagon wrench size 9 64 Alternately loosen ...

Page 223: ...cles may cause damage to the valve and result in poor sealing performance 9 Reinstall the stator and tighten both stator screws alternately each time with approximately one quarter turn until they are tightened Avoid overtightening The screws hold the assembly together and do not affect the sealing force which is automatically set as the screws close the stator against the valve body 10 Reinstall ...

Page 224: ...tridge by using a small screwdriver Fig 84 Fuse cartridge 2 Replace the fuses Warning Always install two fuses Use only the fuses indicated in the following table Avertissement Installez toujours deux nouveaux fusibles Utilisez uniquement les fusibles indiqués ci dessous Description Part No Fuse slow blow 5 x 20 mm NCS 3500RS 4 A NCP 3200RS 2 A Included in the Fuses Kit part no 6820 0026 For infor...

Page 225: ...n updating the firmware in the module from Chromeleon this information will also be provided during the download see further down in this section Whenever a new firmware version is released for the module the new version will be provided with the next Chromeleon Service Release and described in the release notes The new firmware will not be downloaded automatically to the module when you install a...

Page 226: ...not downgrade the firmware Older firmware may be incompatible with new hardware revisions 6 Click Yes to start the download Click No to cancel the action The download may take several minutes The download is complete when Firmware download completed successfully appears in the Messages Server window in the Chromeleon Server Configuration program The message appears also in the Chromeleon Audit Tra...

Page 227: ...fic information about the components in the module For the Find information about the On page NC Pump Interior components detailed view Liquid flow path Operating principle 220 221 222 Loading Pump Interior components detailed view Liquid flow path Operating principle 226 227 228 Column Compartment Interior components Operating principle 229 230 ...

Page 228: ...th Classic flow meter detailed view No Description 1 Leak sensor 2 Detector of the seal wash system 3 Peristaltic pump 4 Purge screw 5 Flow meter inlet 6 Pump lights here hidden by the front panel door 7 Connector for the pressure transducer cable working pressure of the pump head 8 Flow meter outlet 9 Purge outlet 10 Pump head 2 8 1 6 9 10 4 3 7 5 ...

Page 229: ... x 1000 mm I D x L NCP 3200RS 1 0 x 1000 mm ID x L 1 0 x 1300 mm ID x L 6041 2540 6041 2540 6041 2530 2 Pump head with working cylinder and equilibration cylinder entire assembly 6041 1901A 3 Capillary from working cylinder to equilibration cylinder U tube Included in 6041 3002 4 Flow meter page 202 5a Capillary from left pump head to flow meter Included in 6041 3002 5b Capillary from right pump h...

Page 230: ...n 8 1 3 1 ProFlow Flow Meter In the ProFlow flow meter each dual piston pump nos 2a and 2b is controlled by the associated thermal flow sensor nos 5a and 5b The partial flows of these flow controlled pumps nos 1a and 1b are mixed in a Y piece no 6 at the outlet of the flow meter The picture illustrates the functional blocks of the pump with a ProFlow flow meter Fig 87 Functional blocks of the NC p...

Page 231: ...nd 5b Both partial flows are mixed in a Y piece no 7 The pressure at the flow meter outlet no 8 is measured by the column pressure transducer no 6 which is connected to the Y piece 7 by means of a short connection capillary no 9 Both flow restrictors nos 5a and 5b are located in a common flow selector cartridge that can be replaced to select a different flow range The picture illustrates the funct...

Page 232: ...artial flow rates FlSet_A and FlSet_B for both channels from the set total flow rate and the set solvent composition gradient point Fig 89 Operating principle of the pump Classic flow meter In case of the Classic flow meter FlSet_A and FlSet_B are multiplied by the known fluidic resistance RA and RB of the corresponding flow restrictor Then the column pressure PCol is added to obtain the set prima...

Page 233: ...rating principle of the pump ProFlow flow meter In case of the ProFlow flow meter the signals of the flow sensors FlowA and FlowB are compared with the set values F1Set_A and F1Set_B The pumps A and B are controlled in response to the difference between the set values and the sensor signals ...

Page 234: ...pump No Description 1 3 channel proportioning valve 2 Pump block status LED page 146 3 Pump lights here hidden by the front panel door 4 Connector for pressure transducer cable system pressure from purge unit 5 Pump head with working cylinder and equilibration cylinder 6 Purge unit with purge valve and pressure transducer for the system pressure 7 Inline filter 1 3 4 6 7 5 2 ...

Page 235: ...ck of 3 solvent supply lines 6030 2547 2 3 channel proportioning valve 3 Tubing from proportioning valve to pump head 6040 3023 4 Pump head with working cylinder and equilibration cylinder entire assembly 6041 1902 5 Capillary from working cylinder to equilibration cylinder U tube Included in 6041 3001 6 Capillary from pump head to purge unit Included in 6041 3001 7 Purge unit with purge valve and...

Page 236: ...nders successively Continuous delivery is achieved as follows The working cylinder delivers at the appropriate flow rate while simultaneously filling the serially connected equilibration cylinder The latter serves as a reservoir and delivers while the working cylinder carries out the suction stroke The picture illustrates how the pump operates Fig 93 Operating principle of the loading pump No Elem...

Page 237: ...a valve is installed in this position page 19 2 Capillary guides page 60 Capillaries to be routed to the outside on the sides of the column chamber have to be routed through the guides provided on the left and right of the column chamber 3 Column brackets page 80 4 Slots for the column ID chip cards page 129 5 Column switching valve It depends on the configuration of the column compartment whether...

Page 238: ...mponents to the preferred temperature settable in 0 1 C increments Using a heat exchanger they allow fast temperature changes and ensure independence from the ambient temperature All this ensures that The temperature of the stationary phase remains constant over the total column length The column and the solvent have the same temperature during the analysis Under these conditions the analytical se...

Page 239: ...es elbow tubes shut off valves Capillaries for the NC pump nanoViper MP35N Chromeleon software DVD Fitting plugs Viper 6041 3003 Note Operation of the module with a ProFlow flow meter requires a suitable firmware and Chromeleon version Preparations 1 Disconnect the module in Chromeleon 2 Remove the installed flow meter from your module Follow the removal steps in section 7 7 1 Replacing the Flow M...

Page 240: ... Flow Meter page 30 Tip The capillaries can also be used with a Classic flow meter 6 Connect the module in Chromeleon 7 Make sure that the firmware version that is installed on the module is suitable for the ProFlow flow meter If required update the firmware to the firmware shipped in the new Chromeleon version See section 7 14 page 217 8 Open the Chromeleon Server Configuration program and adapt ...

Page 241: ...es See section 4 5 2 Flow Meter Settings page 69 If the solvent that you use is not available in the solvent type list perform a solvent calibration for this solvent See section 5 5 3 1 Performing a Solvent Calibration page 114 Tip To check that all flow connections are tight perform a detailed leak test section 5 7 2 page 134 ...

Page 242: ...low meter Unknown solvents need to be calibrated newly for the ProFlow flow meter See section 5 5 3 1 page 114 When purging the flow meter mind the different purge times for the ProFlow flow meter section 4 5 3 1 2 page 75 The ProFlow flow meter includes a built in inline filter of which you can replace the filter frit For replacement instructions see section 7 7 3 page 205 Different diagnostic an...

Page 243: ... 05 RSD or 0 01 min SD whichever is greater Retention time precision 0 2 RSD or 0 1 min SD whichever is greater for 30 min gradient N a Pressure range ProFlow flow meter 2 90 MPa 290 13050 psi Classic flow meter 2 80 MPa 290 11600 psi at nominal flow Nominal flow for ProFlow flow meter Nano LC complete flow range Classic flow meter Cap LC 5 µL min Micro LC 25 µL min 2 62 MPa 290 9000 psi Pulsation...

Page 244: ...asured at 50 C setpoint Temperature precision 0 1 C Column capacity Maximum available width for column plus fittings 350 mm coiled columns Warm up time from 35 C to 65 C in 12 minutes typically at an ambient temperature of 25 C Column switching valves Up to two 2 position 10 port or 2 position 6 port switching valves Port to port volume 10 port valve 114 nL 6 port valve 91 nL Wetted parts Column s...

Page 245: ... 300 VA max 2 6A 115V 1 3A 230V NCP 3200RS 100 120 V 60 Hz 200 240 V 50 Hz max 150 VA max 1 3A 115V 0 7A 230V Emission sound pressure level 70 dB A in 1 m distance Environmental conditions Range of use Indoor use Temperature 10 C to 35 C 50 to 95 F Air humidity 80 relative humidity non condensing Overvoltage category II Pollution degree 2 Dimensions h w d NCS 3500RS 36 x 42 x 51 cm NCP 3200RS 20 x...

Page 246: ...UltiMate 3000 Series NCS 3500RS and NCP 3200RS Page 238 Operating Instructions ...

Page 247: ...ption Part No Quantity in the kit Accessories kit of the NCS 3500RS including Capillary nanoViper MP35N 0 25 x 155 mm I D x L To be used for example for calibrating solvents with the ProFlow flow meter or establishing the solvent viscosity with the Classic flow meter or for purging the flow meter 6041 7892 1 Chromeleon software DVD 1 Column ID Included in 6710 1505 2 Column installation capillary ...

Page 248: ...S 3500RS NCP 3200RS including 1 open end wrench size 1 4 x 5 16 2 open end wrenches size 11 x 13 mm 1 hexagon wrench size 6 mm 1 piston seal removal and insertion tool 1 pump head tool for RS SD pumps and 1 pump head tool for BM pumps and NCS 3500RS NCP 3200RS the tool is required for establishing the distance during piston installation 6007 9304 1 Tubing connector straight for I D 1 0 2 0 mm Incl...

Page 249: ...70 0026 3 Solvent supply line 1 0 x 1300 mm I D x L 6041 2530 2 Solvent supply line filter including 1 Filter holder top and bottom parts and 1 filter frit PEEK porosity 10 µm 2 spare frits Included in Included in 6268 0115 6268 0117 2 Tool kit for UltiMate 3000 RS SD BM pumps and NCS 3500RS NCP 3200RS including 1 open end wrench size 1 4 x 5 16 2 open end wrenches size 11 x 13 mm 1 hexagon wrench...

Page 250: ...tiMate 3000RSLCnano system can be arranged in different configurations for various applications All parts required for the system setups columns capillaries fittings etc are included in the related RSLCnano application kits For information about how to arrange and set up an RSLCnano System refer to the UltiMate 30000 RSLCnano Standard Applications system manual The manual is shipped with the NCS 3...

Page 251: ... to inline filter 6041 3001 Capillaries capillary kit for NC pump nanoViper MP35N including 2 capillaries from working cylinder to equilibration cylinder U tubes 1 capillary from right pump head to flow meter inlet 1 capillary from left pump head to flow meter inlet 6041 3002 Capillary clips column compartment Column installation capillary clips kit Capillary nanoViper MP35N 0 25 x 155 mm I D x L ...

Page 252: ...only for Capillary LC 0 5 10 µL min Micro LC 5 50 µL min 6041 0003 6041 0014 Fuses kit including 10 fuses 4A slow blow 5 x 20 mm for use in the NCS 10 fuses overload protection 2A slow blow 5 x 20 mm for use in the NCP 5 fuses 4A slow blow 6 3 x 32 mm 6820 0026 Inline filter with filter frit porosity 2 µm for loading pump 6042 5014 Inline filter filter frits Filter frits inline filter Installation...

Page 253: ...r cord Italy 6000 1040 Power cord Japan 6000 1050 Power cord Switzerland 6000 1030 Power cord UK 6000 1020 Power cord US 6000 1001 Pump head entire assembly for NC pump Loading pump 6041 1901A 6041 1902 Purge screw for loading pump 6040 2035 Rear seal wash system reservoir 0 25L including bottle cap 2270 0026 Rear seal wash system seals Fig 65 page 184 nos 4 and 8 PTFE seals 9 x 1 5 mm and 32 x 1 ...

Page 254: ...47 Stator for 2 position 6 port switching valve 2 position 10 port switching valve 6041 0007 6041 0005 Support ring for main piston seal 2 support rings for NC pump and loading pump 6040 0012 Syringe and tubing kit including 5 plastic syringes 3m silicone tubing O D x I D 2 80 mm x 1 30 mm 6000 0010 Tool kit for UltiMate 3000 RS SD BM pumps and NCS 3500RS NCP 3200RS including 1 open end wrench 1 4...

Page 255: ...ures For information about the chemical resistance of PEEK see the table Medium Concentration Temperature Maximum Duration Days Resistance yes no Acetaldehyde techn pure 23 Acetic acid 96 23 7 Acetone 100 23 7 Ammonia 28 23 7 Ammonium sulphate 23 Amyl acetate 100 23 Amyl alcohol techn pure 23 Benzaldehyde 23 7 Benzene 100 23 7 Benzene Benzene mixture 60 42 Benzoic acid 23 Borax 60 Bromine 23 Butan...

Page 256: ...ydrogen peroxide 30 23 7 Lactic acid 23 Magnesium chloride 23 Methanol 100 23 Methyl ethyl ketone 100 23 Methyl isobutyl ketone 100 23 Nitric acid 40 23 7 Nitric acid 65 23 7 Nitrobenzene 100 23 Paraffin oil 60 Paraffin oil 23 Perchlorethylene 100 23 Phenol Diluted 23 Phenol Concentrated 23 Potassium dichromate 23 Potassium hydroxide 23 Potassium nitrate 23 Potassium permanganate 23 Propane 23 Pro...

Page 257: ...ge 249 Medium Concentration Temperature Maximum Duration Days Resistance yes no Sulphuric acid 40 130 Sulphuric acid 50 23 7 Sulphuric acid dissolved 98 23 Toluene 100 23 7 Trichloroethylene 100 23 7 Trichlormethane chloroform 100 23 Water 23 Xylene 100 23 Zinc chloride 23 ...

Page 258: ...tain conditions non miscible liquids may mix or miscible liquids may separate Name Acetone miscible Acetonitrile Benzene non miscible Butanol t Butylmethylether Cyclohexane Cyclopentane Dichloroethane Dichloromethane Di Ethylether Dimethylformamide Dimethyl sulfoxide Dioxane Di Propylether Acetic acid Ethanol Ethyl acetate Heptane Hexane Methanol Methyl ethyl ketone Octane Pentane Propylalcohol Te...

Page 259: ...7 0 33 0 50 2 9 0 76 0 62 1 00 Compressibility χ at 20 C MBar 1 99 97 160 100 123 93 46 Critical Flow Fc mL min 1 13 9 4 14 83 21 18 28 Linear Drop in Pressure Δp l MPa m 2 0 06 0 08 0 06 0 40 0 10 0 10 0 17 Polarity P 3 5 8 3 1 0 1 3 9 5 1 4 0 10 2 1 FC critical flow for 0 25 mm I D tubing FC mL min 113 x 0 25 mm x η cP ρ g mL FC is an example of a hydrodynamic calculation 2 Δ p l linear drop in ...

Page 260: ...he liquid 1 Substances whose flash point is below 38 C are classified as flammable 2 The auto ignition temperature is the lowest temperature at which substances can self ignite at atmospheric pressure without an external ignition source that is without external ignition by sparks or flames The thermal energy required to reach the auto ignition temperature is created by a spontaneous chemical react...

Page 261: ...and Physics 79th Edition CRC Press 1998 1999 5 G W C Kaye and T H Laby Tables of Physical and Chemical Constants 16th Edition Longman Ed 1995 6 Union des Industries Chimiques L Electricité Statique en Atmosphère Explosive Septembre 1982 7 B P Mullins Spontaneous Ignition of Liquid Fuels Butterworths Ed 1955 8 Chemical Safety Sheets Working Safely with Hazardous Chemicals Kluwer Acad Publ Samson Ch...

Page 262: ...UltiMate 3000 Series NCS 3500RS and NCP 3200RS Page 254 Operating Instructions ...

Page 263: ...contact for NO and NC 6 White Relay_NO Potential free Closing contact Fig 96 Pin assignment port and cable Important The maximum switching voltage of the relays is 24 V The switching current must not exceed 100 mA The maximum input voltage at the input must not exceed 5 V with reference to ground The minimum input voltage must not be lower than the ground potential Important La tension maximale de...

Page 264: ...h with Solvent Rack leaks 5 Reserved 6 V_Degas 15V_supply Supply for the solvent rack 7 GND_Degas Ground_supply Reference potential for V_Degas 8 VCC Voltage for logic devices 5V 9 Jumper to pin 3 10 GND Reference potential for VCC 11 GND Reference potential for VCC 12 GND Reference potential for VCC 13 Reserved 14 V_Degas 15V_supply Supply for the solvent rack 15 GND_Degas Ground_supply Reference...

Page 265: ...guration Program 43 45 Server Monitor 43 45 Special Functions 132 USB Driver 43 Chromeleon Dialog Columns 51 Devices 47 Flowmeter 52 General 46 Inputs 52 Limits 48 Oven Valves 50 Pumps 47 Relays 52 Signals 51 Solvents 49 Classic Flow Meter 31 Column Pressure Flow Rate 112 Operating Principle 223 Signals 121 Cleaning Pistons 196 Clear 97 Column Bracket 80 Clips 80 Install 80 Column Compartment 34 7...

Page 266: ... Up 85 Status Screen 86 Display Soft Keys 103 106 Display Filter Level 90 Dock Pistons 191 Door open 27 Drain System 65 E Equilibration 83 Equilibration Time 136 F Filter Level Commands Dialog Box 90 Firmware Download 47 217 Firmware Update 47 217 Firmware Version 103 218 Flow 101 Flow Acceleration 102 119 Flow Deceleration 102 119 Flow Meter 30 202 Settings 69 Flow Meter Configuration 114 Flow Me...

Page 267: ...Interior Components 226 Operating Principle 228 Purge Unit 32 Loading Pump Device 48 M Main Column Compartment Menu 105 Pump Menu 100 Main Device 47 Maintenance 142 Calibration Intervals 144 Internal 142 Intervals 143 Mass Spectrometer Connection 42 Max Pressure 101 MaximumFlowRampDown 119 MaximumFlowRampUp 119 Menu 96 Column Compartment 104 Layout 96 Pump 98 Messages 147 Micro Pump 226 Flow Path ...

Page 268: ...ucer 32 Calibrate 172 Check Offset 172 Pressure Transducer Offset 172 Pressure Transducer Test 134 172 Pressure Unit 103 Prev 97 ProFlow Flow Meter 31 Column Pressure Flow Rate 110 Guidelines after Upgrade 234 Inline Filter Frit Replacement 205 Modification 231 Operating Principle 222 Signals 121 Solvent Calibration 114 Thermal Flow Sensors 110 222 Upgrade 231 Zero Balance Test 172 Program Create ...

Page 269: ...ing 67 180 Piston 184 188 190 196 Piston Seals 184 186 194 195 197 199 Pump Head 184 188 190 195 197 Purge Valve 210 Rotor Seal 214 Safety Precautions 175 Seal Wash System 179 181 199 Tightness Loading Pump 211 Valve Stator 214 Set Flow 95 Shut Down 140 Shut Off Valve 206 Installing 206 Removing 207 Shutdown Program 141 Signals Dialog Box 51 Soft Keys 94 Solvent Compatibility 108 Degasser Compatib...

Page 270: ...gnostics Messages 160 Display Messages 147 Operating Problems 163 Pressure Transducer Offset 172 Zero Balance 172 U Unit Description Configurations 19 Operating Principle 21 Overview 17 Unpacking 37 USB 41 USB Configuration File 44 USB Port 25 V Vacuum Degasser Solvent Compatibility 108 Valve 50 Viper Capillaries 58 Virtual Mode 46 Viscosity Classic Flow Meter Measurement 114 115 135 161 W Wash So...

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