Agilent 1260 Infinity Nanoflow Pump User Manual Agilent Technologies
Notices © Agilent Technologies, Inc. 2007, 2008, 2010 No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws.
Contents Contents 1 Introduction to the 1260 Infinity Nanoflow Pump 7 Introduction to the Pump 8 Early Maintenance Feetback 16 Instrument Layout 17 Electrical Connections 18 Interfaces 20 Setting the 8-bit Configuration Switch (On-Board LAN) 2 Site Requirements and Specifications 26 33 Site Requirements 34 Physical Specifications 37 Performance Specifications 38 3 Installing the Module 41 Unpacking the Module 42 Optimizing the Stack Configuration 44 Installing the Pump 49 Connecting Modules and Cont
Contents 6 Troubleshooting and Diagnostics 79 Overview of the Module’s Indicators and Test Functions Status Indicators 82 User Interfaces 84 Agilent Lab Advisor Software 85 7 Error Information 80 87 What Are Error Messages 89 General Error Messages 90 Module Error Messages 95 8 Test Functions and Calibration 109 Micro Mode Pressure Test 110 Normal Mode Pressure Test 112 Leak Test 116 EMPV Test 124 EMPV Cleaning 125 9 Maintenance 127 Introduction to Maintenance 128 Warnings and Cautions 129 Overvie
Contents 10 Parts and Materials for Maintenance 159 Pump Housing and Main Assemblies 160 Solvent Cabinet and Bottle-Head Assembly Hydraulic Path 164 Pump-Head Assembly 166 Flow Sensor Assembly 168 Nanoflow Pump Accessory Kit 169 11 Identifying Cables 171 Cable Overview 172 Analog Cables 174 Remote Cables 176 BCD Cables 179 CAN/LAN Cables 181 External Contact Cable 182 Agilent Module to PC 183 Agilent 1200 Module to Printer 12 Appendix 163 184 185 General Safety Information 186 The Waste Electrical
Contents 6 1260 Nanoflow Pump User Manual
1260 Nanoflow Pump User Manual 1 Introduction to the 1260 Infinity Nanoflow Pump Introduction to the Pump 8 Hydraulic Path Overview 10 How Does the Pumping Unit Work? 12 How Does Compressibility Compensation Work? How Does Variable Stroke Volume Work? 15 Early Maintenance Feetback Instrument Layout 14 16 17 Electrical Connections 18 Serial Number Information (ALL) Rear View of the Module 19 Interfaces 20 Overview Interfaces 18 22 Setting the 8-bit Configuration Switch (On-Board LAN) Communication Se
1 Introduction to the 1260 Infinity Nanoflow Pump Introduction to the Pump Introduction to the Pump The low flow pumps consist of two identical pumping units in a single housing. They generate gradients by high-pressure mixing. A solvent selection valve provides flexibility in the choice of solvents. Mobile phase composition is produced by mixing the outputs of pumphead A and B. The solvent selection valve allows the pumphead A output to originate from either channel A1 or channel A2.
Introduction to the 1260 Infinity Nanoflow Pump Introduction to the Pump 1 EdlZg hjeean 8HB WdVgY Ejbe Yg^kZ 9VbeZg B^mZg ;Vc DjiaZi kVakZ Ejbe ]ZVY 6 ;adl hZchdg 6Xi^kZ ^caZi kVakZ Ejbe ]ZVY 7 AZV` hZchdg cdi ^chiVaaZY HdakZci hZaZXi^dc kVakZ Figure 1 Overview of the Pump 1260 Nanoflow Pump User Manual 9
1 Introduction to the 1260 Infinity Nanoflow Pump Introduction to the Pump Hydraulic Path Overview The NanoFlow Pump is based on the 1200 Series Binary Pump (pressure limit 400 bar, active inlet valves), and performs all the functions necessary for a µ-flow solvent delivery system.
Introduction to the 1260 Infinity Nanoflow Pump Introduction to the Pump 1 9Z\VhhZg ;gdb hdakZci WdiiaZ ;gdb hdakZci WdiiaZ Ejbe ]ZVY 6 Ejbe ]ZVY 7 E^hidc HZVa >caZi kVakZ DjiaZi kVakZ B^m^c\ X]VbWZg DjiaZi kVakZ >caZi kVakZ :BEK 9VbeZg ;adl hZchdg ;^aiZg Id lVhiZ Figure 2 The Hydraulic Path of the NanoFlow Pump 1260 Nanoflow Pump User Manual 11
1 Introduction to the 1260 Infinity Nanoflow Pump Introduction to the Pump How Does the Pumping Unit Work? Both pumping units (channel A and channel B) are identical with respect to parts and function. Each pumping unit consists of a pump head which is directly attached to a metering drive assembly. In each metering drive assembly, a servo-controlled variable reluctance motor and gear train assembly are used to move two ball-screw drives.
Introduction to the 1260 Infinity Nanoflow Pump Introduction to the Pump 1 closes the outlet valve, preventing any chamber 2 solvent from back-streaming into chamber 1. After a predefined piston 1 stroke length, the servo motor is stopped, and the active inlet valve is closed. The pistons now reverse directions. Piston 1 begins its delivery stroke (high pressure), and piston 2 begins its intake stroke. Piston 2 is moving at only half the speed of piston 1.
1 Introduction to the 1260 Infinity Nanoflow Pump Introduction to the Pump Table 1 Pump Details Materials in contact with mobile phase Pump head SST, gold, sapphire, ceramic Active inlet valve SST, gold, sapphire, ruby, ceramic, PTFE Outlet valve SST, gold, sapphire, ruby, tantalum Adapter SST, gold EMPV SST, ruby, sapphire, PEEK Flow sensor SST Damping unit Gold, SST Capillaries Fused silica For pump specifications, see “Performance Specifications” on page 38.
1 Introduction to the 1260 Infinity Nanoflow Pump Introduction to the Pump How Does Variable Stroke Volume Work? Due to the compression of the pump-chamber volume each piston stroke of the pump will generate a small pressure pulsation, influencing the flow ripple of the pump. The amplitude of the pressure pulsation is mainly dependent on the stroke volume and the compressibility compensation for the solvent in use.
1 Introduction to the 1260 Infinity Nanoflow Pump Early Maintenance Feetback Early Maintenance Feetback Maintenance requires the exchange of components which are subject to wear or stress. Ideally, the frequency at which components are exchanged should be based on the intensity of usage of the module and the analytical conditions, and not on a predefined time interval.
Introduction to the 1260 Infinity Nanoflow Pump Instrument Layout 1 Instrument Layout The industrial design of the module incorporates several innovative features. It uses Agilent’s E-PAC concept for the packaging of electronics and mechanical assemblies. This concept is based upon the use of expanded polypropylene (EPP) layers of foam plastic spacers in which the mechanical and electronic boards components of the module are placed.
1 Introduction to the 1260 Infinity Nanoflow Pump Electrical Connections Electrical Connections • The CAN bus is a serial bus with high speed data transfer. The two connectors for the CAN bus are used for internal module data transfer and synchronization. • One analog output provides signals for integrators or data handling systems.
Introduction to the 1260 Infinity Nanoflow Pump Electrical Connections 1 Rear View of the Module 8dc[^\jgVi^dc hl^iX] Hadi [dg ^ciZg[VXZ WdVgY GH'(' GZbdiZ 6cVad\ djieji 86C"7jh EdlZg Eaj\ HZXjg^in AZkZg Figure 4 NOTE Rear View of the Module The GPIB interface has been removed with the introduction of the 1260 Infinity modules.
1 Introduction to the 1260 Infinity Nanoflow Pump Interfaces Interfaces The Agilent 1200 Infinity Series modules provide the following interfaces: Table 2 Agilent 1200 Infinity Series Interfaces Module CAN LAN/BCD (optional) LAN (on-board) RS-232 Analog APG Remote Special G1310B Iso Pump G1311B Quat Pump G1311C Quat Pump VL G1312B Bin Pump G1312C Bin Pump VL 1376A Cap Pump G2226A Nano Pump 2 Yes No Yes 1 Yes G4220A/B Bin Pump 2 No Yes Yes No Yes G1361A Prep Pump 2 Yes No Yes
1 Introduction to the 1260 Infinity Nanoflow Pump Interfaces Table 2 Agilent 1200 Infinity Series Interfaces Module CAN LAN/BCD (optional) LAN (on-board) RS-232 Analog APG Remote Special G4212A/B DAD 2 No Yes Yes 1 Yes G1315C DAD VL+ G1365C MWD G1315D DAD VL G1365D MWD VL 2 No Yes Yes 2 Yes G1321B FLD G1362A RID 2 Yes No Yes 1 Yes G4280A ELSD No No No Yes Yes Yes G1316A/C TCC 2 No No Yes No Yes G1322A DEG No No No No No Yes AUX G1379B DEG No No No Ye
1 Introduction to the 1260 Infinity Nanoflow Pump Interfaces Overview Interfaces CAN The CAN is inter-module communication interface. It is a 2-wire serial bus system supporting high speed data communication and real-time requirement. LAN The modules have either an interface slot for an LAN card (e.g. Agilent G1369A/B LAN Interface) or they have an on-board LAN interface (e.g. detectors G1315C/D DAD and G1365C/D MWD).
1 Introduction to the 1260 Infinity Nanoflow Pump Interfaces The RS-232C is designed as DCE (data communication equipment) with a 9-pin male SUB-D type connector.
1 Introduction to the 1260 Infinity Nanoflow Pump Interfaces APG Remote The APG Remote connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features as common shut down, prepare, and so on. Remote control allows easy connection between single instruments or systems to ensure coordinated analysis with simple coupling requirements. The subminiature D connector is used.
Introduction to the 1260 Infinity Nanoflow Pump Interfaces Table 4 1 Remote Signal Distribution Pin Signal Description 1 DGND Digital ground 2 PREPARE (L) Request to prepare for analysis (for example, calibration, detector lamp on). Receiver is any module performing pre-analysis activities. 3 START (L) Request to start run / timetable. Receiver is any module performing run-time controlled activities. 4 SHUT DOWN (L) System has serious problem (for example, leak: stops pump).
1 Introduction to the 1260 Infinity Nanoflow Pump Setting the 8-bit Configuration Switch (On-Board LAN) Setting the 8-bit Configuration Switch (On-Board LAN) The 8-bit configuration switch is located at the rear of the module. Switch settings provide configuration parameters for LAN, serial communication protocol and instrument specific initialization procedures. All modules with on-board LAN, e.g.
Introduction to the 1260 Infinity Nanoflow Pump Setting the 8-bit Configuration Switch (On-Board LAN) Table 5 1 8-bit Configuration Switch (with on-board LAN) Mode Function SW 1 SW 2 0 0 LAN SW 3 SW 4 SW 5 SW 6 Link Configuration SW 7 SW 8 Init Mode Selection Auto-negotiation 0 x x x x x 10 MBit, half-duplex 1 0 0 x x x 10 MBit, full-duplex 1 0 1 x x x 100 MBit, half-duplex 1 1 0 x x x 100 MBit, full-duplex 1 1 1 x x x Bootp x x x 0 0 0 Bootp & Stor
1 Introduction to the 1260 Infinity Nanoflow Pump Setting the 8-bit Configuration Switch (On-Board LAN) Setting the 8-bit Configuration Switch (without On-Board LAN) The 8-bit configuration switch is located at the rear of the module. Modules that do not have their own LAN interface (e.g. the TCC) can be controlled through the LAN interface of another module and a CAN connection to that module.
1 Introduction to the 1260 Infinity Nanoflow Pump Setting the 8-bit Configuration Switch (On-Board LAN) Table 6 NOTE 8-bit Configuration Switch (without on-board LAN) Mode Select 1 2 RS-232C 0 1 Reserved 1 0 TEST/BOOT 1 1 3 4 5 Baudrate 6 7 Data Bits 8 Parity Reserved RSVD SYS RSVD RSVD FC The LAN settings are done on the LAN Interface Card G1369A/B. Refer to the documentation provided with the card.
1 Introduction to the 1260 Infinity Nanoflow Pump Setting the 8-bit Configuration Switch (On-Board LAN) Table 8 Baudrate Settings (without on-board LAN) Switches Baud Rate 3 4 5 0 0 0 0 0 0 0 Table 9 Switches Baud Rate 3 4 5 9600 1 0 0 9600 1 1200 1 0 1 14400 1 0 2400 1 1 0 19200 1 1 4800 1 1 1 38400 Data Bit Settings (without on-board LAN) Switch 6 Data Word Size 0 7 Bit Communication 1 8 Bit Communication Table 10 Parity Settings (without on-board LAN)
Introduction to the 1260 Infinity Nanoflow Pump Setting the 8-bit Configuration Switch (On-Board LAN) 1 Special Settings The special settings are required for specific actions (normally in a service case). NOTE The tables include both settings for modules – with on-board LAN and without on-board LAN. They are identified as LAN and no LAN. Boot-Resident Firmware update procedures may require this mode in case of firmware loading errors (main firmware part).
1 Introduction to the 1260 Infinity Nanoflow Pump Setting the 8-bit Configuration Switch (On-Board LAN) Forced Cold Start A forced cold start can be used to bring the module into a defined mode with default parameter settings. CAUTION Loss of data Forced cold start erases all methods and data stored in the non-volatile memory. Exceptions are diagnosis and repair log books which will not be erased. ➔ Save your methods and data before executing a forced cold start.
1260 Nanoflow Pump User Manual 2 Site Requirements and Specifications Site Requirements 34 Physical Specifications 37 Performance Specifications 38 This chapter provides information about site requirements, physical specifications and performance specifications of the 1260 Infinity Nanoflow Pump.
2 Site Requirements and Specifications Site Requirements Site Requirements A suitable environment is important to ensure optimal performance of the instrument. Power Considerations The module power supply has wide ranging capability. It accepts any line voltage in the range described in Table 13 on page 37. Consequently there is no voltage selector in the rear of the module. There are also no externally accessible fuses, because automatic electronic fuses are implemented in the power supply.
2 Site Requirements and Specifications Site Requirements Power Cords Different power cords are offered as options with the module. The female end of all power cords is identical. It plugs into the power-input socket at the rear. The male end of each power cord is different and designed to match the wall socket of a particular country or region.
2 Site Requirements and Specifications Site Requirements Bench Space The module dimensions and weight (see Table 13 on page 37) allow you to place the module on almost any desk or laboratory bench. It needs an additional 2.5 cm (1.0 inches) of space on either side and approximately 8 cm (3.1 inches) in the rear for air circulation and electric connections. If the bench should carry an Agilent system, make sure that the bench is designed to bear the weight of all modules.
2 Site Requirements and Specifications Physical Specifications Physical Specifications Table 13 Physical Specifications Type Specification Weight 17 kg (38 lbs) Dimensions (height × width × depth) 180 x 345 x 435 mm (7 x 13.
2 Site Requirements and Specifications Performance Specifications Performance Specifications Table 14 Performance Specification Agilent 1260 Infinity Nano Pump (G2226A) Type Specification Hydraulic system Two independent pump channels, each with two pistons in series. One proprietary servo-controlled variable stroke drive per channel.
Site Requirements and Specifications Performance Specifications Table 14 2 Performance Specification Agilent 1260 Infinity Nano Pump (G2226A) Type Specification Analog output For pressure monitoring, 2 mV/bar, one output Communications Controller-area network (CAN), RS-232C, APG Remote: ready, start, stop and shut-down signals, LAN optional Safety and maintenance Extensive diagnostics, error detection and display (though Instant Pilot and Data System), leak detection, safe leak handling, leak outp
2 40 Site Requirements and Specifications Performance Specifications 1260 Nanoflow Pump User Manual
1260 Nanoflow Pump User Manual 3 Installing the Module Unpacking the Module 42 Delivery Checklist 42 Nanoflow Pump Accessory Kit Optimizing the Stack Configuration One Stack Configuration 44 Two Stack Configuration 47 Installing the Pump 43 44 49 Connecting Modules and Control Software 52 Connecting Modules 52 Connecting a Vacuum Degasser 52 Connecting Control Software and/or G4208 A Instant Pilot Flow Connections 53 54 Get the System Ready for the First Injection 58 Manually Priming the Solvent Chan
3 Installing the Module Unpacking the Module Unpacking the Module If the delivery packaging shows signs of external damage, please call your Agilent Technologies sales and service office immediately. Inform your service representative that the instrument may have been damaged during shipment. CAUTION "Defective on arrival" problems If there are signs of damage, please do not attempt to install the module. Inspection by Agilent is required to evaluate if the instrument is in good condition or damaged.
Installing the Module Unpacking the Module Table 15 3 Nano Pump Checklist Description Quantity 1260 Nanoflow Pump (G2226-64050) 1 HPLC Tool Kit (optional) (p/n G4203-68708) 1 LC HW User Information + Utilities DVD (p/n 4800-64005) 1 Accessory Kit On-Line Degasser (p/n G1379-68705 ) 1 Nanoflow Pump Accessory Kit Accessory Kit (Nano Pump) (p/n G2226-68755) p/n Description 01018-60025 (4x) Solvent inlet filter, stainless steel 0515-0175 Mounting screw for manual purge valve holder, M4, 20 mm
3 Installing the Module Optimizing the Stack Configuration Optimizing the Stack Configuration If your module is part of a complete Agilent 1260 Infinity Liquid Chromatograph, you can ensure optimum performance by installing the following configurations. These configurations optimize the system flow path, ensuring minimum delay volume.
Installing the Module Optimizing the Stack Configuration 3 HdakZci XVW^cZi KVXjjb YZ\VhhZg Ejbe AdXVa JhZg >ciZg[VXZ 6jidhVbeaZg 8dajbc XdbeVgibZci 9ZiZXidg Figure 8 Recommended Stack Configuration for 1260 (Front View) 1260 Nanoflow Pump User Manual 45
3 Installing the Module Optimizing the Stack Configuration GZbdiZ XVWaZ 86C 7jh XVWaZ id adXVa jhZg ^ciZg[VXZ 68 edlZg 86C 7jh XVWaZ 6cVad\ YZiZXidg h^\cVa & dg ' djiejih eZg YZiZXidg A6C id A8 8]ZbHiVi^dc adXVi^dc YZeZcYh dc YZiZXidg Figure 9 46 Recommended Stack Configuration for 1260 (Rear View) 1260 Nanoflow Pump User Manual
Installing the Module Optimizing the Stack Configuration 3 Two Stack Configuration To avoid excessive height of the stack when the autosampler thermostat is added to the system it is recommended to form two stacks. Some users prefer the lower height of this arrangement even without the autosampler thermostat. A slightly longer capillary is required between the pump and autosampler. (See Figure 10 on page 47 and Figure 11 on page 48).
3 Installing the Module Optimizing the Stack Configuration A6C id Xdcigda hd[ilVgZ 86C 7jh XVWaZ id >chiVci E^adi I]Zgbd XVWaZ dei^dcVa 68 EdlZg GZbdiZ XVWaZ 68 EdlZg 86C 7jh XVWaZ 68 EdlZg Figure 11 48 Recommended Two Stack Configuration for 1260 (Rear View) 1260 Nanoflow Pump User Manual
Installing the Module Installing the Pump 3 Installing the Pump Parts required # p/n 1 Pump 1 1 Description Data System G4208A 1 Instant Pilot Power cord For other cables see text below and “Cable Overview” on page 172. Preparations WA R N I N G • • • Locate bench space. Provide power connections. Unpack the module. Module is partially energized when switched off, as long as the power cord is plugged in. Repair work at the module can lead to personal injuries, e.g.
3 Installing the Module Installing the Pump 1 Place the module on the bench in a horizontal position. 2 Ensure the power switch at the front of the module is OFF (switch stands out). HiVijh aVbe EdlZg hl^iX] HZg^Va cjbWZg Figure 12 Front View of the Module 3 At the rear of the module move the security lever to its maximum right position. 4 Connect the power cable to the power connector at the rear of the module.
Installing the Module Installing the Pump 3 5 Connect the required interface cables to the rear of the pump, see “Connecting Modules” on page 52. 8dc[^\jgVi^dc hl^iX] Hadi [dg ^ciZg[VXZ WdVgY GH'(' GZbdiZ 6cVad\ djieji 86C"7jh EdlZg Eaj\ HZXjg^in AZkZg Figure 13 Rear View of the Module 6 Connect the capillary, solvent tubes and waste line (see “Flow Connections” on page 54). 7 Press the power switch to turn on the module.
3 Installing the Module Connecting Modules and Control Software Connecting Modules and Control Software WA R N I N G Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury. ➔ Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
3 Installing the Module Connecting Modules and Control Software Connecting Control Software and/or G4208 A Instant Pilot NOTE With the introduction of the Agilent 1260 Infinity, all GPIB interfaces have been removed. The preferred communication is LAN. NOTE Usually the detector is producing the most data in the stack, followed by the pump, and it is therefore highly recommended to use either of these modules for the LAN connection.
3 Installing the Module Flow Connections Flow Connections Parts required # p/n 1 WA R N I N G Other modules 1 G1376-68755 Accessory Kit 1 G2226-68755 Accessory Kit (Nano Pump) 2 Preparations Description wrenches 1/4 - 5/16 inch for capillary connections Pump is installed in the LC system When opening capillary or tube fittings solvents may leak out. The handling of toxic and hazardous solvents and reagents can bear health risks.
Installing the Module Flow Connections 3 1 Remove the front cover by pressing the snap fasteners on both sides. Figure 14 Removing the Front Cover 2 Place the solvent cabinet on top of the module. 3 Remove the sintered glas inlet filters and the filter adapters from the bottle head assemblies. Replace them by the stainless steel filters from the pump asseccories kit. NOTE Use a piece of sand paper to get a good grip when pushing the stainless steel filters into the tubings.
3 Installing the Module Flow Connections 7 Purge your system before first use (see “Priming Your System With the Pump” on page 59).
Installing the Module Flow Connections 1 Capillary EMPV to Nano Flow sensor (4 µL flow sensor) (p/n G1375-87321) 2 Capillary, damper to mixer (capillary pump only) (p/n 01090-87308) 3 Capillary, filter to EMPV (p/n G1375-87400) 4 Fused Silica/PEEK capillary 25 µm, 35 cm (p/n G1375-87322) 5 Restriction capillary (p/n G1312-67304) 6 Mixing capillary (p/n G1312-67302) 7 Connecting tube, SSV to AIV (p/n G1311-67304) 8 Bottle-head assembly (p/n G1311-60003) 1260 Nanoflow Pump User Manual 3 57
3 Installing the Module Get the System Ready for the First Injection Get the System Ready for the First Injection When you are using the system for the first time it is recommended to prime it to remove all the air and the possible contamination introduced in the flow path during the installation. NOTE The pump should never be used for priming empty tubings (never let the pump run dry).
3 Installing the Module Get the System Ready for the First Injection 7 Repeat steps 4 to 6 for the three remaining solvent channels. 8 When all 4 channels are manually primed, remove the paper towel from the pump leak tray. Make sure that the pump leak sensor is dry before turning on the pump. Priming Your System With the Pump WA R N I N G When opening capillary or tube fittings solvents may leak out. The handling of toxic and hazardous solvents and reagents can bear health risks.
3 60 Installing the Module Get the System Ready for the First Injection 1260 Nanoflow Pump User Manual
1260 Nanoflow Pump User Manual 4 Using the Pump Hints For Successfully Using the Pump Solvent Information 62 64 Algae Growth in HPLC Systems 65 How to Prevent and/or Reduce the Algae Problem Checkout procedure for a G2229A Nano LC System Method Parameters 68 Test Results and Evaluation 70 66 67 This chapter provides advice for the successful operation of the 1260 Series Nanoflow Pump and the checkout procedure for Agilent capillary HPLC-systems.
4 Using the Pump Hints For Successfully Using the Pump Hints For Successfully Using the Pump Pump Issues • Flush the pump extensively. First with in the Purge Mode, second with a pressure applied to remove all the gas bubbles. It is recommended to do this first with 100 % A and than 100 % B. • The system pressure must be higher than 20 bar at the pump outlet. • In Micro Mode, unexpected high column flow variation is an indication for dirt within the system, blocked frits or leaking pump valves.
4 Using the Pump Hints For Successfully Using the Pump Fused Silica Capillary Issues • When connecting a capillary (especially at the column) press it smoothly into the fitting to avoid void volumes. Incorrect setting will result in dispersion, causing tailing or footing peaks. NOTE The quartz core of PEEK/fused silica capillaries will crack and debris will clog the flow path if the fittings are overtightened. Fittings shouldn't be tightened harder than finger tight plus 1/4 turn with a wrench.
4 Using the Pump Solvent Information Solvent Information Always filter solvents through 0.4 µm filters, small particles can permanently block the capillaries and valves. Avoid the use of the following steel-corrosive solvents: • Solutions of alkali halides and their respective acids (for example, lithium iodide, potassium chloride, and so on).
4 Using the Pump Algae Growth in HPLC Systems Algae Growth in HPLC Systems The presence of algae in HPLC systems can cause a variety of problems that may be incorrectly diagnosed as instrument or application problems. Algae grow in aqueous media, preferably in a pH range of 4-8. Their growth is accelerated by buffers, for example phosphate or acetate. Since algae grow through photosynthesis, light will also stimulate their growth. Even in distilled water small-sized algae grow after some time.
4 Using the Pump Algae Growth in HPLC Systems • Algae growth may also be the possible source for failures of the ball valves and other components in the flow path. How to Prevent and/or Reduce the Algae Problem • Always use freshly prepared solvents, especially use demineralized water which was filtered through about 0.2 µm filters. • Never leave mobile phase in the instrument for several days without flow. • Always discard old mobile phase.
Using the Pump Checkout procedure for a G2229A Nano LC System 4 Checkout procedure for a G2229A Nano LC System Use this procedure to confirm that • the system has been installed correctly • the Nanoflow LC System performs within specification • a technical problem is caused by the Nanoflow LC System Parts required Preparations # Description G1379B 1260 Micro Degasser G2226A 1260 Nanoflow Pump G1377A 1260 Micro High Performance Autosampler G2226-67300 Nanoflow restriction capillary • • • Chan
4 Using the Pump Checkout procedure for a G2229A Nano LC System 8 Pump 0.6 µL/min, micro mode, 70 % A (water) / 30 % B (acetonitrile). Pump as long as it takes for the pressure to become stable. Pump at least 5 min more before continuing. NOTE Make absolutely sure that all parts of the flow path have been thoroughly flushed before starting the checkout procedure. Any trace of other solvents, air bubbles or leaks in the flow path will negatively affect the results.
Using the Pump Checkout procedure for a G2229A Nano LC System Table 17 Time (min) 4 Timetable 0.00 Flow 0.6 (µL/mi n) 3.00 3.01 6.00 6.01 9.00 9.01 12.00 12.01 15.00 0.6 0.3 0.3 0.6 0.6 0.3 0.3 0.6 0.6 Method Parameters Micro High Performance Autosampler • Injection volume: 0.000 µL • Injection mode: Edit inj. prog. (→Inject + →Bypass) NOTE Verify that the injection valve is set to Mainpass in the Set Injection Valve box of the Autosampler Configuration dialog.
4 Using the Pump Checkout procedure for a G2229A Nano LC System Test Results and Evaluation Typical pressure in bypass mode at 600 nL/min is 100 bar and at 300 nL/min50 bar (with the Fused Silica/PEEK capillary 25 µm, 35 cm (p/n G1375-87322) installed between the flow sensor and port 1 of the injection valve plus the restriction capillary installed on port 6 of the injection valve).
1260 Nanoflow Pump User Manual 5 Optimizing Performance Hints for the Micro Vacuum Degasser Choosing the Right Pump Seals How to Choose the Primary Flow The Standard Filter 72 73 74 75 How to Optimize the Compressibility Compensation Setting 76 This chapter provides additional information about further application specific hardware and parameter optimization.
5 Optimizing Performance Hints for the Micro Vacuum Degasser Hints for the Micro Vacuum Degasser If you are using the vacuum degasser for the first time, if the vacuum degasser was switched off for any length of time (for example, overnight), or if the vacuum degasser lines are empty, you should prime the vacuum degasser before running an analysis. The vacuum degasser can be primed by pumping solvent with the 1260 Nanoflow Pump at high flow rate (2.5 mL/min).
Optimizing Performance Choosing the Right Pump Seals 5 Choosing the Right Pump Seals The standard seal for the pump can be used for most applications. However applications that use normal phase solvents (for example, hexane) are not suited for the standard seal and require a different seal when used for a longer time in the pump.
5 Optimizing Performance How to Choose the Primary Flow How to Choose the Primary Flow The primary flow can be set in three ranges: • The default range The default range is the best compromise between performance and solvent consumption. • The low solvent consumption range The low solvent consumption range, is recommended for long shallow gradient runs (e.g. peptide maps) or isocratic operation. This mode is not suitable for fast changes in solvent composition due to the longer gradient delay.
Optimizing Performance The Standard Filter 5 The Standard Filter The standard filter has a volume of typically 100 µL. If the application needs a reduced volume (e.g. for fast gradient), the use of the Universal solvent filter kit, 20 µL (p/n 01090-68703) is recommended. Be aware that the filter efficiency and capacity is significantly reduced compared to the standard one. NOTE Never run the pump without an inline filter.
5 Optimizing Performance How to Optimize the Compressibility Compensation Setting How to Optimize the Compressibility Compensation Setting The compressibility compensation default settings are 50 × 10-6 /bar (best for most aqueous solutions) for pump head A and 115 × 10-6 /bar (to suit organic solvents) for pump head B. The settings represent average values for aqueous solvents (A side) and organic solvents (B side).
5 Optimizing Performance How to Optimize the Compressibility Compensation Setting 5 Starting with a compressibility setting of 10 × 10-6 /bar increase the value in steps of 10. Re-zero the integrator as required. The compressibility compensation setting that generates the smallest pressure ripple is the optimum value for your solvent composition. 6 Repeat step 1 on page 76 through step 5 on page 77 for the B channel of your pump.
5 78 Optimizing Performance How to Optimize the Compressibility Compensation Setting 1260 Nanoflow Pump User Manual
1260 Nanoflow Pump User Manual 6 Troubleshooting and Diagnostics Overview of the Module’s Indicators and Test Functions 80 Status Indicators 82 Power Supply Indicator 82 Module Status Indicator 83 User Interfaces 84 Agilent Lab Advisor Software 85 This chapter provides information about the module's status indicators, error messages, and the available test functions in Instant Pilot and Lab Advisor.
6 Troubleshooting and Diagnostics Overview of the Module’s Indicators and Test Functions Overview of the Module’s Indicators and Test Functions Status Indicators The module is provided with two status indicators which indicate the operational state (prerun, run, and error states) of the module. The status indicators provide a quick visual check of the operation of the module.
6 Troubleshooting and Diagnostics Overview of the Module’s Indicators and Test Functions Leak Rate Test The Leak Rate Test is a diagnostic test designed to determine the pressure tightness of the pump. When a problem with the pump is suspected, use this test to help troubleshoot the pump and its pumping performance. EMPV Test The EMPV test is designed to verify the performance of the EMPV. Perform this test after replacing the EMPV or when observing flow stability problems in micro mode.
6 Troubleshooting and Diagnostics Status Indicators Status Indicators Two status indicators are located on the front of the module. The lower left indicates the power supply status, the upper right indicates the module status. HiVijh ^cY^XVidg \gZZc$nZaadl$gZY A^cZ edlZg hl^iX] l^i] \gZZc a^\]i Figure 16 Location of Status Indicators Power Supply Indicator The power supply indicator is integrated into the main power switch. When the indicator is illuminated (green) the power is ON.
6 Troubleshooting and Diagnostics Status Indicators Module Status Indicator The module status indicator indicates one of six possible module conditions: • When the status indicator is OFF (and power switch light is on), the module is in a prerun condition, and is ready to begin an analysis. • A green status indicator, indicates the module is performing an analysis (run mode). • A yellow indicator indicates a not-ready condition.
6 Troubleshooting and Diagnostics User Interfaces User Interfaces Depending on the User Interface, the available tests vary. Some descriptions are only available in the Service Manual. Table 20 84 Test Functions available vs.
Troubleshooting and Diagnostics Agilent Lab Advisor Software 6 Agilent Lab Advisor Software The Agilent Lab Advisor software is a standalone product that can be used with or without data system. Agilent Lab Advisor software helps to manage the lab for high quality chromatographic results and can monitor in real time a single Agilent LC or all the Agilent GCs and LCs configured on the lab intranet. Agilent Lab Advisor software provides diagnostic capabilities for all Agilent 1200 Infinity Series modules.
6 86 Troubleshooting and Diagnostics Agilent Lab Advisor Software 1260 Nanoflow Pump User Manual
1260 Nanoflow Pump User Manual 7 Error Information What Are Error Messages 89 General Error Messages 90 Timeout 90 Shut-Down 90 Remote Timeout 91 Synchronization Lost 91 Leak Sensor Short 92 Leak Sensor Open 92 Compensation Sensor Open Compensation Sensor Short Fan Failed 94 Leak 94 93 93 Module Error Messages 95 Zero Solvent Counter 95 Pressure Above Upper Limit 95 Pressure Below Lower Limit 96 Pressure Signal Missing 96 Valve Failed 97 Missing Pressure Reading 98 Pump Configuration 98 Valve Fuse 99 I
7 Error Information Agilent Lab Advisor Software Flow Sensor Missing 103 Leak Sensor Missing 103 Servo Restart Failed 104 Pump Head Missing 105 Index Limit 105 Index Adjustment 106 Index Missing 106 Stroke Length 107 Initialization Failed 107 Wait Timeout 108 Electronic fuse of SSV 108 This chapter describes the meaning of error messages, and provides information on probable causes and suggested actions how to recover from error conditions.
7 Error Information What Are Error Messages What Are Error Messages Error messages are displayed in the user interface when an electronic, mechanical, or hydraulic (flow path) failure occurs which requires attention before the analysis can be continued (for example, repair, or exchange of consumables is necessary). In the event of such a failure, the red status indicator at the front of the module is switched on, and an entry is written into the module logbook.
7 Error Information General Error Messages General Error Messages General error messages are generic to all Agilent series HPLC modules and may show up on other modules as well. Timeout The timeout threshold was exceeded. Probable cause Suggested actions 1 The analysis was completed successfully, Check the logbook for the occurrence and source of a not-ready condition. Restart the analysis where required. and the timeout function switched off the module as requested.
7 Error Information General Error Messages Remote Timeout A not-ready condition is still present on the remote input. When an analysis is started, the system expects all not-ready conditions (for example, a not-ready condition during detector balance) to switch to run conditions within one minute of starting the analysis. If a not-ready condition is still present on the remote line after one minute the error message is generated.
7 Error Information General Error Messages Leak Sensor Short The leak sensor in the module has failed (short circuit). The current through the leak sensor is dependent on temperature. A leak is detected when solvent cools the leak sensor, causing the leak-sensor current to change within defined limits. If the current increases above the upper limit, the error message is generated. Probable cause Suggested actions 1 Defective flow sensor. Please contact your Agilent service representative.
Error Information General Error Messages 7 Compensation Sensor Open The ambient-compensation sensor (NTC) on the main board in the module has failed (open circuit). The resistance across the temperature compensation sensor (NTC) on the main board is dependent on ambient temperature. The change in resistance is used by the leak circuit to compensate for ambient temperature changes. If the resistance across the sensor increases above the upper limit, the error message is generated.
7 Error Information General Error Messages Fan Failed The cooling fan in the module has failed. The hall sensor on the fan shaft is used by the main board to monitor the fan speed. If the fan speed falls below a certain limit for a certain length of time, the error message is generated. Probable cause Suggested actions 1 Fan cable disconnected. Please contact your Agilent service representative. 2 Defective fan. Please contact your Agilent service representative. 3 Defective main board.
Error Information Module Error Messages 7 Module Error Messages Zero Solvent Counter The error message is triggered if the remaining volume in a solvent bottle falls below the set limit. Probable cause Suggested actions 1 Volume in bottle below specified volume. Refill bottles and reset solvent counters. 2 Incorrect setting. Make sure the set solvent volume matches the actual bottle filling and set the shutoff limit to a reasonable value (e.g.
7 Error Information Module Error Messages Pressure Below Lower Limit The system pressure has fallen below the lower pressure limit. Probable cause Suggested actions 1 Solvent bottle empty. Replenish solvent. 2 Lower pressure limit set too high. Ensure the lower pressure limit is set to a value suitable for the analysis. 3 Leak. • Inspect the pump head, capillaries and fittings for signs of a leak. • Purge the module.
Error Information Module Error Messages 7 Valve Failed Valve 0 Failed: valve A1 Valve 1 Failed: valve A2 Valve 2 Failed: valve B2 Valve 3 Failed: valve B1 One of the solvent selection valves in the module failed to switch correctly. The processor monitors the valve voltage before and after each switching cycle. If the voltages are outside expected limits, the error message is generated. Probable cause Suggested actions 1 Solvent selection valve disconnected.
7 Error Information Module Error Messages Missing Pressure Reading The pressure readings read by the pump ADC (analog-digital converter) are missing. The ADC reads the pressure signal of from the damper every 1ms. If the readings are missing for longer than 10 seconds, the error message is generated. Probable cause Suggested actions 1 Damper disconnected. Please contact your Agilent service representative. 2 Defective damper. Please contact your Agilent service representative.
Error Information Module Error Messages 7 Valve Fuse Valve Fuse 0: Channels A1 and A2 Valve Fuse 1: Channels B1 and B2 One of the solvent-selection valves in the pump has drawn excessive current causing the selection-valve electronic fuse to open. Probable cause Suggested actions 1 Defective solvent selection valve. Restart the capillary pump. If the error message appears again, exchange the solvent selection valve.
7 Error Information Module Error Messages Temperature Out of Range Temperature Out of Range 0: Pump channel A Temperature Out of Range 1: Pump channel B One of the temperature sensor readings in the motor-drive circuit are out of range. The values supplied to the ADC by the hybrid sensors must be between 0.5 V and 4.3 V. If the values are outside this range, the error message is generated. Probable cause Suggested actions 1 Defective main board. Please contact your Agilent service representative.
7 Error Information Module Error Messages Motor-Drive Power The current drawn by the pump motor exceeded the maximum limit. Blockages in the flow path are usually detected by the pressure sensor in the damper, which result in the pump switching off when the upper pressure limit is exceeded. If a blockage occurs before the damper, the pressure increase cannot be detected by the pressure sensor and the module will continue to pump. As pressure increases, the pump drive draws more current.
7 Error Information Module Error Messages Encoder Missing The optical encoder on the pump motor in the module is missing or defective. The processor checks the presence of the pump encoder connector every 2 seconds. If the connector is not detected by the processor, the error message is generated. Probable cause Suggested actions 1 Defective or disconnected pump encoder Please contact your Agilent service representative. connector. 2 Defective pump drive assembly.
Error Information Module Error Messages 7 Electro-Magnetic-Proportional-Valve (EMPV) Missing EMPV Missing The EMPV in the capillary pump or nanoflow pump is missing or defective. Probable cause Suggested actions 1 Disconnected or defective cable. Please contact your Agilent service representative. 2 Defective solenoid. Exchange the solenoid of the EMPV. Flow Sensor Missing Probable cause Suggested actions 1 Flow sensor disconnected. Ensure the sensor is seated correctly.
7 Error Information Module Error Messages Servo Restart Failed The pump motor in the module was unable to move into the correct position for restarting. When the module is switched on, the first step is to switch on the C phase of the variable reluctance motor. The rotor should move to one of the C positions. The C position is required for the servo to be able to take control of the phase sequencing with the commutator.
7 Error Information Module Error Messages Pump Head Missing The pump-head end stop in the pump was not found. When the pump restarts, the metering drive moves forward to the mechanical end stop. Normally, the end stop is reached within 20 seconds, indicated by an increase in motor current. If the end point is not found within 20 seconds, the error message is generated. Probable cause Suggested actions 1 Pump head not installed correctly (screws Install the pump head correctly. Ensure nothing (e.g.
7 Error Information Module Error Messages Index Adjustment The encoder index position in the module is out of adjustment. During initialization, the first piston is moved to the mechanical stop. After reaching the mechanical stop, the piston reverses direction until the encoder index position is reached. If the time to reach the index position is too long, the error message is generated. Probable cause Suggested actions 1 Irregular or sticking drive movement.
Error Information Module Error Messages 7 Stroke Length The distance between the lower piston position and the upper mechanical stop is out of limits (pump). During initialization, the module monitors the drive current. If the piston reaches the upper mechanical stop position before expected, the motor current increases as the module attempts to drive the piston beyond the mechanical stop. This current increase causes the error message to be generated.
7 Error Information Module Error Messages Wait Timeout When running certain tests in the diagnostics mode or other special applications, the pump must wait for the pistons to reach a specific position, or must wait for a certain pressure or flow to be reached. Each action or state must be completed within the timeout period, otherwise the error message is generated. Possible Reasons for a Wait Timeout: · Pressure not reached. · Pump channel A did not reach the delivery phase.
1260 Nanoflow Pump User Manual 8 Test Functions and Calibration Micro Mode Pressure Test 110 Running the Test from the Agilent Lab Advisor Software Micro Mode Pressure Test Results 111 110 Normal Mode Pressure Test 112 Positioning the Blank Nut 113 Running the Pressure Test 114 Evaluating the Results 115 Leak Test 116 Leak Test Description 116 Running the Leak Test 118 Evaluating the Results 119 EMPV Test 124 EMPV Test Description 124 Running the EMPV Test 124 EMPV Cleaning 125 1260 Nanoflow Pump EMPV Cl
8 Test Functions and Calibration Micro Mode Pressure Test Micro Mode Pressure Test Description This is a fast test to verify the tightness of a micro system, where the pump is operating in Micro Mode and no manual purge valve is installed. The flow path of the system which is tested for tightness is blocked by a blank nut. The pressure is increased up to 380 bar and the remaining flow is measured with the flow sensor while the system is blocked.
8 Test Functions and Calibration Micro Mode Pressure Test Micro Mode Pressure Test Results The test results are evaluated automatically. The sum of all leaks within the column flow path from the EMPV to the blank nut must be lower than 100 nL/min. NOTE Small leaks, with no visible leaks in the flow path can cause the test to fail. If the pressure test fails Ensure all fittings between the pump and the blank nut are tight and repeat the pressure test.
8 Test Functions and Calibration Normal Mode Pressure Test Normal Mode Pressure Test Description The System Pressure Test is a quick, built-in test designed to demonstrate the pressure-tightness of the system. The test is required, if problems with small leaks are suspected, or after maintenance of flow-path components (e.g., pump seals, injection seal) to prove pressure tightness up to 400 bar. For running the test, please refer to the online help of the diagnostic software.
Test Functions and Calibration Normal Mode Pressure Test 8 Positioning the Blank Nut If a specific component is suspected of causing a system leak, place the blank nut immediately before the suspected component, then run the Pressure Test again. If the test passes, the defective component is located after the blank nut. Confirm the diagnosis by placing the blank nut immediately after the suspected component. The diagnosis is confirmed if the test fails.
8 Test Functions and Calibration Normal Mode Pressure Test Running the Pressure Test When • • Tools required Wrench 1/4 inch Parts required # p/n 1 01080-83202 1 Preparations NOTE • • • If problems with small leaks are suspected After maintenance of flow-path components (e.g. pump seals, injection seal) to prove pressure tightness up to 400 bar bar. Description Blank nut 500 ml Isopropanol Place a bottle of LC-grade isopropanol in the solvent cabinet and connect it to channel A2.
Test Functions and Calibration Normal Mode Pressure Test 8 Evaluating the Results The sum of all leaks between the pump and the blank nut will be indicated by a pressure drop of >2 bar/minute at the plateau. Note that small leaks may cause the test to fail, but solvent may not be seen leaking from a module. NOTE Please notice the difference between an error in the test and a failure of the test! An error means that during the operation of the test there was an abnormal termination.
8 Test Functions and Calibration Leak Test Leak Test Leak Test Description The Leak Test is a built-in troubleshooting test designed to demonstrate the leak-tightness of the pump. The test involves monitoring the pressure profile as the pump runs through a predefined pumping sequence. The resulting pressure profile provides information about the pressure tightness and operation of the pump components. Ramp 1 The test begins with the initialization of both pumps.
Test Functions and Calibration Leak Test 8 Plateau 2 Piston B2 delivers with a flow rate of 3 µL/min for 30 s. Ramp 5 Piston A1 delivers 50 µL/min for approximately 8 s. Plateau 3 Piston A1 delivers with a flow rate of 3 µL/min for 30 s. Ramp 6 Piston B1 delivers 50 µL/min for approximately 7 s. Plateau 4 Piston B1 delivers with a flow rate of 3 µL/min for approximately 30 s. At the end of the fourth plateau, the test is finished and the pump switches off.
8 Test Functions and Calibration Leak Test Running the Leak Test When If problems with the pump are suspected Tools required Wrench 1/4 inch Parts required # p/n Description 1 G1313-87305 Restriction Capillary 1 01080-83202 1 Preparations • • • NOTE Blank nut 500 ml Isopropanol Place two bottles of LC-grade isopropyl alcohol in channels A2 and B2. The EMPV is not designed for pressure tightness towards the waste port. Install the manual purge valve from the accessories kit to pump head A.
8 Test Functions and Calibration Leak Test Evaluating the Results Defective or leaky components in the pump head lead to changes in the Leak Test pressure plot. Typical failure modes are described below. NOTE Please notice the difference between an error in the test and a failure of the test! An error means that during the operation of the test there was an abnormal termination. If a test failed, this means that the results of the test were not within the specified limits.
8 Test Functions and Calibration Leak Test Pressure limit not reached but plateaus horizontal or positive Probable cause Suggested actions 1 Degasser and pump channels A and/or B Purge the degasser and pump channels thoroughly with isopropanol under pressure (use the restriction capillary). not flushed sufficiently (air in the channels). 2 Wrong solvent. Install isopropanol. Purge the degasser and pump channels thoroughly.
8 Test Functions and Calibration Leak Test First plateau negative or unstable, and at least one other plateau positive Probable cause Suggested actions 1 Leaking outlet valve in channel A. Clean the outlet valve in channel A. Ensure the sieve in the outlet valves are installed correctly. Tighten the outlet valve. 2 Loose pump head screws in channel A. Ensure the pump head screws in channel A are tight. 3 Leaking seal or scratched piston in channel Exchange the pump seals in channel A.
8 Test Functions and Calibration Leak Test Third plateau negative or unstable and at least one other plateau positive Probable cause Suggested actions 1 Air in channel A or new seals not yet seated. Flush channel A thoroughly with isopropanol under pressure (use restriction capillary). 2 Loose active inlet valve in channel A. Tighten the active inlet valve in channel A (14 mm wrench). Do not overtighten! 3 Loose pump head screws in channel A. Ensure the pump head screws in channel A are tight.
8 Test Functions and Calibration Leak Test Fourth plateau negative or unstable and at least one other plateau positive Probable cause Suggested actions 1 Air in pump chamber of channel B or seals Flush channel B thoroughly with isopropanol under pressure (restriction capillary). not yet seated. 2 Loose active inlet valve in channel B. Tighten the active inlet valve in channel B (14mm wrench). Do not overtighten! 3 Loose pump head screws in channel B.
8 Test Functions and Calibration EMPV Test EMPV Test EMPV Test Description The test is designed to verify the performance of the EMPV. The test must always be done when the EMPV valve is exchanged. The test should also be done if column flow stability problems occur (micro mode only). The EMPV test is not a substitute for the leak test or pressure test. The leak and pressure tests should also be done when leaks within the pump heads might be the problem.
8 Test Functions and Calibration EMPV Cleaning EMPV Cleaning 1260 Nanoflow Pump EMPV Cleaning Description Depending on the application, particles can sometimes collect in the EMPV. This fast cleaning routine is designed to remove such particle deposits. The routine should always be performed when the EMPV is suspected of being leaky or contaminated with particles. The outlet of the EMPV is plugged with an SST blank nut.
8 126 Test Functions and Calibration EMPV Cleaning 1260 Nanoflow Pump User Manual
1260 Nanoflow Pump User Manual 9 Maintenance Introduction to Maintenance Warnings and Cautions 129 Overview of Maintenance Cleaning the Module 128 130 132 Early Maintenance Feedback (EMF) EMF Counters 134 Using the EMF Counters 135 133 Checking and Cleaning the Solvent Inlet Filters 136 Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve Removing the Active Inlet Valve 138 Exchanging the Valve Cartridge 139 Replacing the Active Inlet Valve Body 140 Exchanging the Outlet Valve Si
9 Maintenance Introduction to Maintenance Introduction to Maintenance The pump is designed for easy repair. The most frequent repairs such as piston seal exchange and filter frit replacement can be done with the pump in place in the system stack. These repairs are described in Table 23 on page 130.
9 Maintenance Warnings and Cautions Warnings and Cautions WA R N I N G Toxic, flammable and hazardous solvents, samples and reagents The handling of solvents, samples and reagents can hold health and safety risks. ➔ When working with these substances observe appropriate safety procedures (for example by wearing goggles, safety gloves and protective clothing) as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice.
9 Maintenance Overview of Maintenance Overview of Maintenance Table 23 Simple Repair Procedures Procedure Symptom Notes “Removing the Active Inlet Valve” on page 138 If internally leaking Pressure ripple unstable, run leak test for verification “Exchanging the Outlet Valve Sieve” on page 142 If internally leaking Pressure ripple unstable, run leak test for verification “Exchanging the Solvent Selection Valve” on page 144 Unstable column flow or system pressure “Exchanging the Solvent Selecti
9 Maintenance Overview of Maintenance * + , ) - ( .
9 Maintenance Cleaning the Module Cleaning the Module The module case should be kept clean. Cleaning should be done with a soft cloth slightly dampened with water or a solution of water and mild detergent. Do not use an excessively damp cloth as liquid may drip into the module. WA R N I N G Liquid dripping into the electronic compartment of your module. Liquid in the module electronics can cause shock hazard and damage the module. ➔ Do not use an excessively damp cloth during cleaning.
Maintenance Early Maintenance Feedback (EMF) 9 Early Maintenance Feedback (EMF) Maintenance requires the exchange of components in the flow path which are subject to mechanical wear or stress. Ideally, the frequency at which components are exchanged should be based on the intensity of usage of the instrument and the analytical conditions, and not on a predefined time interval.
9 Maintenance Early Maintenance Feedback (EMF) EMF Counters The pump provides a series of EMF counters for the pump head. Each counter increments with pump use, and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded. Each counter can be reset to zero after maintenance has been done. The pump provides the following EMF counters: • liquimeter pump A, • seal wear pump A, • liquimeter pump B, • seal wear pump B.
Maintenance Early Maintenance Feedback (EMF) 9 Using the EMF Counters The user-settable EMF limits for the EMF counters enable the early maintenance feedback to be adapted to specific user requirements. The wear of pump components is dependent on the analytical conditions, therefore, the definition of the maximum limits need to be determined based on the specific operating conditions of the instrument.
9 Maintenance Checking and Cleaning the Solvent Inlet Filters Checking and Cleaning the Solvent Inlet Filters When If solvent filter is blocked Parts required Description Concentrated nitric acid (65 %) Bidistilled water Beaker Preparations WA R N I N G Remove the solvent inlet tube from the inlet port of the solvent selection valve or the adapter at the active inlet valve When opening capillary or tube fittings solvents may leak out.
9 Maintenance Checking and Cleaning the Solvent Inlet Filters Cleaning the Solvent Filters 1 Remove the blocked solvent filter from the bottle-head assembly and place it in a beaker with concentrated nitric acid (35%) for one hour. 2 Thoroughly flush the filter with LC grade water (remove all nitric acid, some columns can be damaged by concentrated nitric acid). 3 Reinstall the filter.
9 Maintenance Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve Removing the Active Inlet Valve When If defective, see next two procedures for repair details.
Maintenance Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve 9 Exchanging the Valve Cartridge When If internally leaking (backflow) Tools required Wrench 14 mm Parts required # p/n Description 1 5062-8562 Active Inlet Valve Cartridge (400 bar) 1 Using a pair of tweezers remove the valve cartridge from the actuator assembly. 2 Before inserting the new valve cartridge clean the area in the actuator assembly. Fill a syringe with alcohol and flush the cartridge area thoroughly.
9 Maintenance Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve Replacing the Active Inlet Valve Body When • • If leaking from the bottom of the active inlet valve body If the soleniod is defective Tools required Wrench 14 mm Parts required # Description G1312-60025 Active inlet valve without cartridge 5062-8562 Active Inlet Valve Cartridge (400 bar), optional 1 Move the AIV cartridge from the old valve body to the new one. Optionally, you may use a new AIV cartridge.
Maintenance Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve 9 6 After an exchange of the valve cartridge it may be required to prime the respective pump channel with several milliliters of solvent before it is completely purged and the pressure ripple has returned to its normal value.
9 Maintenance Exchanging the Outlet Valve Sieve Exchanging the Outlet Valve Sieve When Sieve — whenever the pump seals will be exchanged Valve — if internally leaking Tools required Wrench 1/4 inch Wrench 14 mm Parts required NOTE # p/n Description 1 G1312-60067 Outlet valve, complete 1 5063-6505 Sieve (pack of 10) Before exchanging the outlet valve you can try to clean it in a sonic bath. Remove the gold seal and the sieve.
Maintenance Exchanging the Outlet Valve Sieve 9 6 Check that the new valve is assembled correctly and that the gold seal is present (if the gold seal is deformed, it should be replaced). KVakZ WdYn
9 Maintenance Exchanging the Solvent Selection Valve Exchanging the Solvent Selection Valve When If leaking internally, if blocked or if one of the solenoids is defective Tools required Screwdriver Pozidriv #1 Parts required # Description G1312-60068 Solvent selection valve CAUTION Solvent spillage ➔ Position the solvent bottles at a level below the pump to avoid solvent spillage due to hydrostatic pressure.
9 Maintenance Exchanging the Solvent Selection Valve 1 Disconnect the solvent tubes and the active inlet valve connection tubes from the solvent selection valves. Place solvent tubes into the solvent cabinet to prevent leaks due to hydrostatic flow. HdakZci ijWZh HdakZci hZaZXi^dc kVakZ 8dccZXi^c\ ijWZh Figure 22 Exchanging the solvent selection valve 2 Using a Pozidriv screwdriver #1 loosen the holding screws of the valves. 3 Pull the valve module out and detach the connector.
9 Maintenance Removing and Disassembling the Pump Head Removing and Disassembling the Pump Head When • • • Exchanging pump seals Exchanging pistons Exchanging seals of the seal wash option Tools required Wrench 1/4 inch 3-mm hexagonal key 4-mm hexagonal key Preparations CAUTION • • Switch off pump at power switch Remove the front cover to have access to the pump mechanics Damage of the pump drive Starting the pump when the pump head is removed may damage the pump drive.
Maintenance Removing and Disassembling the Pump Head 3 Place the pump head on a flat surface. Loosen the lock screw (two revolutions). While holding the lower half of the assembly, carefully pull the pump head away from the piston housing. Ejbe ]ZVY 9 4 Remove the support rings from the piston housing and lift the housing away from the pistons.
9 Maintenance Exchanging the Pump Seals and Seal Wear-in Procedure Exchanging the Pump Seals and Seal Wear-in Procedure When Seals leaking, if indicated by the results of the pump test (check both pump heads individually!) Tools required 3-mm hexagonal key 4-mm hexagonal key 1/4 inch wrench Parts required # p/n Description 2 5063-6589 (standard) or 0905-1420 (for normal phase application) Seals (pack of 2) 1 5022-2159 Restriction capillary 1 Disassemble the pump head assembly of the leaky p
Maintenance Exchanging the Pump Seals and Seal Wear-in Procedure 3 Clean the pump chambers with lint free cloth. Ensure all particulate matter is removed. Best cleaning results will be achieved by removing all valves (see “Removing the Active Inlet Valve” on page 138 and “Exchanging the Outlet Valve Sieve” on page 142) and the capillary. Inject solvent into each chamber. 8]VbWZgh 9 4 Insert seals into the pump head and press firmly in position.
9 Maintenance Exchanging the Pump Seals and Seal Wear-in Procedure Seal Wear-in Procedure NOTE This procedure is required for standard seals only (5063-6589), but it will definitely damage the normal phase application seals (0905-1420). 1 Place a bottle with 100 ml of Isopropanol in the solvent cabinet and place the tubing (including bottle head assembly) of the pump head that is supposed to be worn-in into the bottle.
9 Maintenance Exchanging the Pistons Exchanging the Pistons When When scratched Tools required • • Parts required # p/n Description 1 5063-6586 Piston 3-mm hexagonal key 4-mm hexagonal key 1 Disassemble the pump head assembly (see “Removing and Disassembling the Pump Head” on page 146) 2 Check the piston surface and remove any deposits or layers. Cleaning can be done with alcohol or tooth paste. Replace piston if scratched.
9 Maintenance Exchanging the Pistons 3 Reassemble the pump head assembly (see “Reassembling the Pump Head Assembly” on page 154).
Maintenance Exchanging the Flow Sensor 9 Exchanging the Flow Sensor When Extended flow range (100 ul) needed. Leak on the flow sensor. Unstable column flow Flow sensor blocked Tools required Screwdriver Pozidriv #1 Parts required # p/n Description 1 G1376-60004 Nano Flow Sensor 4 µL (1260 Nanoflow Pump) 1 Turn off the pump. 2 Using a 1/4 inch wrench disconnect the capillaries: • coming from the EMPV. • going to the injection device (port 1). 3 Unscrew the flow sensor. 4 Re-install the new one.
9 Maintenance Reassembling the Pump Head Assembly Reassembling the Pump Head Assembly Tools required • • • 3-mm hexagonal key 4-mm hexagonal key PTFE lubricant (79846-65501) 1 Place the support rings on the piston housing (pistons not 2 Tighten the lock screw. installed) and snap the pump head and piston housing together.
9 Maintenance Reassembling the Pump Head Assembly 3 Carefully insert the pistons into the pump head assembly 4 Slide the pump head assembly onto the pump drive. Apply and press them completely into the seals. E^hidc a small amount of pump head grease to the pumphead screws and the balls of the spindle drive. Tighten screws stepwise with increasing torque. 7Vaah d[ he^cYaZ Yg^kZ Ejbe ]ZVY VhhZbWan Ejbe ]ZVY hXgZlh 5 Reconnect the capillaries, tubing and the active inlet valve cable to the connector.
9 Maintenance Exchanging the Optional Interface Board Exchanging the Optional Interface Board When Board defective Parts required # Description 1 BCD (Interface) board CAUTION Electronic boards are static sensitive and should be handled with care so as not to damage them. Touching electronic boards and components can cause electrostatic discharge (ESD). ESD can damage electronic boards and components. ➔ Be sure to hold the board by the edges and do not touch the electrical components.
Maintenance Replacing Module Firmware 9 Replacing Module Firmware When The installation of newer firmware might be necessary • if a newer version solves problems of older versions or • to keep all systems on the same (validated) revision. The installation of older firmware might be necessary • to keep all systems on the same (validated) revision or • if a new module with newer firmware is added to a system or • if third part control software requires a special version.
9 158 Maintenance Replacing Module Firmware 1260 Nanoflow Pump User Manual
1260 Nanoflow Pump User Manual 10 Parts and Materials for Maintenance Pump Housing and Main Assemblies 160 Solvent Cabinet and Bottle-Head Assembly Hydraulic Path 163 164 Pump-Head Assembly 166 Flow Sensor Assembly 168 Nanoflow Pump Accessory Kit 169 This chapter provides information on parts for maintenance.
10 Parts and Materials for Maintenance Pump Housing and Main Assemblies Pump Housing and Main Assemblies Repair Parts — Pump Housing and Main Assemblies (Front View) Item p/n Description 1 G1312-60064 Pump Head without Seal Wash 2 G1311-60001 Pump drive assembly G1311-69001 Exchange assembly for pump drive 3 G1311-61601 Cable assembly — AIV to main board 4 G2226-65030 Nanoflow pump main board (NPM) G2226-69030 Exchange assembly - NPM board G4280-81618 Cable assembly—solvent selection va
Parts and Materials for Maintenance Pump Housing and Main Assemblies 10 ) ( ' * &% + , && & cdi ^chiVaaZY .
10 Parts and Materials for Maintenance Pump Housing and Main Assemblies Repair Parts—Pump Housing and Main Assemblies (Rear View) Item p/n Description 1 1251-7788 Hexagonal Nut for remote/RS-232 connector 2 2940-0256 Nut M14 — analog output 3 0515-0910 Screw M4 x 0.7, 8 mm lg, to fix power supply at rear panel 4 0515-0924 Screw M3x0.
Parts and Materials for Maintenance Solvent Cabinet and Bottle-Head Assembly 10 Solvent Cabinet and Bottle-Head Assembly Item p/n Description 1 5065-9981 Solvent cabinet, including all plastic parts 2 5042-8901 Name plate 5043-0207 Name plate 1260 3 5065-9954 Front panel, solvent cabinet 4 5042-8567 Leak pan G1311-60003 Bottle-head assembly 5/6 01018-60025 Solvent inlet filter, stainless steel 7 5062-2483 Solvent tubing, 5 m 5063-6598 Ferrules with lock ring (10x) 5063-6599 Tube
10 Parts and Materials for Maintenance Hydraulic Path Hydraulic Path Item p/n Description 1 G1311-60003 Bottle-head assembly 2 G1311-67304 Connecting tube, SSV to AIV 3 G1312-67300 Capillary, outlet valve to piston 2 4 G1312-67304 Restriction capillary 5 G1312-67302 Mixing capillary 9 5064-8273 Filter assembly (includes frit) 5022-2185 Replacement SS frit, 0.
Parts and Materials for Maintenance Hydraulic Path 10 [gdb YZ\VhhZg , + && - &' &% ( * ( ) ' .
10 Parts and Materials for Maintenance Pump-Head Assembly Pump-Head Assembly Item p/n Description G1312-60064 Pump Head without Seal Wash 1 5067-4695 Sapphire piston (default) 2 G1312-60062 Adapter, integrated, 1260 3 G4220-63015 Support Ring without Seal Wash G4220-24013 Backup Ring for Seal Holder 5063-6589 Seal, general purpose, black, pack of 2 0905-1420 Seal, general purpose, black, pack of 2 5 G1312-67300 Capillary, outlet valve to piston 2 6 G1312-25260 Pump head body, 1260
Parts and Materials for Maintenance Pump-Head Assembly * 10 && &% .
10 Parts and Materials for Maintenance Flow Sensor Assembly Flow Sensor Assembly p/n Description G1375-60004 NanoFlow sensor 4 µL G1375-87321 Capillary EMPV to Nano Flow sensor (4 µL flow sensor) G1375-87323 Capillary NanoFlow sensor to injection device (4 µL flow sensor), 25 µm ID, 55 cm length & Figure 29 168 Flow Sensor Assembly 1260 Nanoflow Pump User Manual
Parts and Materials for Maintenance Nanoflow Pump Accessory Kit 10 Nanoflow Pump Accessory Kit Accessory Kit (Nano Pump) (p/n G2226-68755) p/n Description 01018-60025 (4x) Solvent inlet filter, stainless steel 0515-0175 Mounting screw for manual purge valve holder, M4, 20 mm long 0890-1760 Tubing Flexible, 2 m 2190-0586 Washer for purge valve holder screw 5022-2185 Replacement SS frit, 0.
10 Parts and Materials for Maintenance Nanoflow Pump Accessory Kit 170 1260 Nanoflow Pump User Manual
1260 Nanoflow Pump User Manual 11 Identifying Cables Cable Overview 172 Analog Cables 174 Remote Cables 176 BCD Cables 179 CAN/LAN Cables 181 External Contact Cable Agilent Module to PC 182 183 Agilent 1200 Module to Printer 184 This chapter provides information on cables used with the Agilent 1200 Infinity Series modules.
11 Identifying Cables Cable Overview Cable Overview NOTE Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
Identifying Cables Cable Overview 11 CAN cables p/n Description 5181-1516 CAN cable, Agilent module to module, 0.
11 Identifying Cables Analog Cables Analog Cables One end of these cables provides a BNC connector to be connected to Agilent modules. The other end depends on the instrument to which connection is being made.
Identifying Cables Analog Cables 11 Agilent Module to BNC Connector p/n 8120-1840 Pin BNC Pin Agilent module Signal Name Shield Shield Analog - Center Center Analog + Pin Agilent module Signal Name Agilent Module to General Purpose p/n 01046-60105 Pin 3394/6 1 1260 Nanoflow Pump User Manual Not connected 2 Black Analog - 3 Red Analog + 175
11 Identifying Cables Remote Cables Remote Cables One end of these cables provides a Agilent Technologies APG (Analytical Products Group) remote connector to be connected to Agilent modules. The other end depends on the instrument to be connected to.
Identifying Cables Remote Cables 11 Agilent Module to 3396 Series III / 3395B Integrators p/n 03396-61010 Pin 33XX Pin Agilent module Signal Name 9 1 - White Digital ground NC 2 - Brown Prepare run Low 3 3 - Gray Start Low NC 4 - Blue Shut down Low NC 5 - Pink Not connected NC 6 - Yellow Power on High 14 7 - Red Ready High 4 8 - Green Stop Low NC 9 - Black Start request Low 13, 15 Active (TTL) Not connected Agilent Module to Agilent 35900 A/D Converters p/n 5061-33
11 Identifying Cables Remote Cables Agilent Module to General Purpose p/n 01046-60201 178 Pin Universal Pin Agilent module Signal Name Active (TTL) 1 - White Digital ground 2 - Brown Prepare run Low 3 - Gray Start Low 4 - Blue Shut down Low 5 - Pink Not connected 6 - Yellow Power on High 7 - Red Ready High 8 - Green Stop Low 9 - Black Start request Low 1260 Nanoflow Pump User Manual
Identifying Cables BCD Cables 11 BCD Cables One end of these cables provides a 15-pin BCD connector to be connected to the Agilent modules.
11 Identifying Cables BCD Cables Agilent Module to 3396 Integrators p/n 03396-60560 180 Pin 3396 Pin Agilent module Signal Name BCD Digit 1 1 BCD 5 20 2 2 BCD 7 80 3 3 BCD 6 40 4 4 BCD 4 10 5 5 BCD0 1 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 +5V Low 1260 Nanoflow Pump User Manual
Identifying Cables CAN/LAN Cables 11 CAN/LAN Cables Both ends of this cable provide a modular plug to be connected to Agilent modules CAN or LAN connectors. CAN Cables p/n Description 5181-1516 CAN cable, Agilent module to module, 0.
11 Identifying Cables External Contact Cable External Contact Cable 5 10 15 1 6 11 One end of this cable provides a 15-pin plug to be connected to Agilent modules interface board. The other end is for general purpose.
Identifying Cables Agilent Module to PC 11 Agilent Module to PC p/n Description G1530-60600 RS-232 cable, 2 m RS232-61600 RS-232 cable, 2.5 m Instrument to PC, 9-to-9 pin (female). This cable has special pin-out, and is not compatible with connecting printers and plotters. It's also called "Null Modem Cable" with full handshaking where the wiring is made between pins 1-1, 2-3, 3-2, 4-6, 5-5, 6-4, 7-8, 8-7, 9-9.
11 Identifying Cables Agilent 1200 Module to Printer Agilent 1200 Module to Printer 184 p/n Description 5181-1529 Cable Printer Serial & Parallel, is a SUB-D 9 pin female vs. Centronics connector on the other end (NOT FOR FW UPDATE). For use with G1323 Control Module.
1260 Nanoflow Pump User Manual 12 Appendix General Safety Information 186 The Waste Electrical and Electronic Equipment Directive Batteries Information Radio Interference Sound Emission 189 190 191 192 Solvent Information 193 Agilent Technologies on Internet 194 This chapter provides addition information on safety, legal and web.
12 Appendix General Safety Information General Safety Information The following general safety precautions must be observed during all phases of operation, service, and repair of this instrument. Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design, manufacture, and intended use of the instrument. Agilent Technologies assumes no liability for the customer’s failure to comply with these requirements.
Appendix General Safety Information 12 Make sure that only fuses with the required rated current and of the specified type (normal blow, time delay, and so on) are used for replacement. The use of repaired fuses and the short-circuiting of fuse holders must be avoided. Some adjustments described in the manual, are made with power supplied to the instrument, and protective covers removed. Energy available at many points may, if contacted, result in personal injury.
12 Appendix General Safety Information Safety Symbols Table 24 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect risk of harm to the operator and to protect the apparatus against damage. Indicates dangerous voltages. Indicates a protected ground terminal. Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in this product.
Appendix The Waste Electrical and Electronic Equipment Directive 12 The Waste Electrical and Electronic Equipment Directive Abstract The Waste Electrical and Electronic Equipment (WEEE) Directive (2002/96/EC), adopted by EU Commission on 13 February 2003, is introducing producer responsibility on all electric and electronic appliances starting with 13 August 2005. NOTE This product complies with the WEEE Directive (2002/96/EC) marking requirements.
12 Appendix Batteries Information Batteries Information WA R N I N G Lithium batteries may not be disposed-off into the domestic waste. Transportation of discharged Lithium batteries through carriers regulated by IATA/ICAO, ADR, RID, IMDG is not allowed. Danger of explosion if battery is incorrectly replaced. ➔ Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries.
Appendix Radio Interference 12 Radio Interference Cables supplied by Agilent Technologies are screened to provide optimized protection against radio interference. All cables are in compliance with safety or EMC regulations. Test and Measurement If test and measurement equipment is operated with unscreened cables, or used for measurements on open set-ups, the user has to assure that under operating conditions the radio interference limits are still met within the premises.
12 Appendix Sound Emission Sound Emission Manufacturer’s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991. This product has a sound pressure emission (at the operator position) < 70 dB.
Appendix Solvent Information 12 Solvent Information Observe the following recommendations on the use of solvents. • Brown glass ware can avoid growth of algae. • Small particles can permanently block capillaries and valves. Therefore always filter solvents through 0.4 µm filters.
12 Appendix Agilent Technologies on Internet Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at: http://www.agilent.com Select Products/Chemical Analysis It will provide also the latest firmware of the modules for download.
Index Index 8 8-bit configuration switch on-board LAN 26 without On-Board LAN buffer application 62 C 28 A active inlet valve 130, 138, 138 Agilent Diagnostic software 85 Agilent Lab Advisor software 85 Agilent Lab Advisor 85 Agilent on internet 194 algae 193 alternative seal material 73 ambient operating temperature 37 ambient non-operating temperature 37 analog output 39 analog signal 23 analog cable 174 apg remote 24 AUTO mode 15 AUX output 52 B battery safety information 190 BCD board 156 BCD cab
Index EMPV test 124 EMPV cleaning 81 encoder missing 102 error messages fan failed 94 error messages compensation sensor open 93 compensation sensor short 93 encoder missing 102 index adjustment 106 index limit 105 index missing 106 initialization failed 107 inlet-valve fuse 99 inlet-valve missing 102 leak sensor open 92 leak sensor short 92 leak 94 missing pressure reading 98 motor drive power 101 pressure above upper limit 95 pressure below lower limit 96 pump head missing 105 remote timeout 91 selection
Index remote timeout 91 missing pressure reading 98 motor-drive power 101 N non-operating altitude 37 non-operating temperature 37 O operating Altitude 37 operating temperature 37 optimization stack configuration 44 outlet valve 130, 142 overview pump 10 P packaging damaged 42 parts main assemblies 160 parts identification cables 171 parts bottle head assembly 163 flow sensor 168 hydraulic path 164 pump head 166 pump housing 160 solvent cabinet 163 performance specification 38 pH range 38 physical speci
Index rear view 48 status indicator 83 stroke length 107 stroke volume 15 synchronization lost 91 system setup and installation optimizing stack configuration wrench 1/4 inch 146 Z zero solvent counter 95 44 T temperature limit exceeded 100 temperature out of range 100 temperature sensor 94 test functions 80 timeout 90 tools screwdriver pozidriv #1 148 screwdriver pozidriv #1 144, 153 wrench 1/4 inch 148 troubleshooting error messages 80, 89 status indicators 80, 82 V vacuum degasser 52 variable str
www.agilent.com In This Book This manual contains technical reference information about the Agilent 1260 Infinity Nanoflow Pump (G2226A). The manual describes the following: • introduction to the pump, • requirements and specifications, • installation, • using the pump, • optimizing performance, • troubleshooting and diagnostics, • maintenance, • parts and materials, • overview of cables, • legal, safety and warranty information.
