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G1376-90014 - Agilent Technologies

1. Figure 13 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 Use a piece of sand paper to get a good grip when pushing the stainless steel filters into the tubings 4 Connect the bottle head solvent tubes to the lower ports of the online degasser Connect the upper ports of the online degasser to the inlet ports Al A2 B1 and B2 of the solvent selection valve of the pump Fix the solvent tubes in the clips of pump degasser and solvent cabinet Label the solvent tubings with the provided stick on labels 5 Using a piece of emery cloth connect the waste tubing to the EMPV and place it into your waste system 6 Ifthe pump is not part of an Agilent 1260 Infinity system stack or placed on the bottom of a stack connect the corrugated waste tube to the waste outlet of the pump leak handling system 1260 Capillary Pump User Manual 55 3 Installing the Module Flow Connections 7 Purge your system before first use see Priming Your System With the Pump on page 59 1 2 5 To port 1 of the injection valve Waste Pump head A Pump head B Figure 14 Flow connection of the capillary pump 56 1260 Capillary Pump User Manual Installing the Module 3 1 Capillary EMPV to flow sensor 20 uL flow sensor p n
2. 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 elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 61376 90014 Edition 06 2010 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn This product may be used as a com ponent of an in vitro diagnostic sys tem if the system is registered with the appropriate authorities and com plies with the relevant regulations Otherwise it is intended only for gen eral laboratory use Warranty The material contained in this docu ment is provided as is and is sub ject to being changed without notice in future editions Further to the max imum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or perfor mance of this document or of any information contained herein Should Agilent and the user have a separat
3. Make sure to release the pressure by slowly opening the purge valve when the test has finished Evaluating the Results on page 123 describes the evaluation and interpretation of the leak test results For detailed instructions refer to the Agilent Lab Advisor software Tool 1260 Capillary Pump User Manual Test Functions and Calibration 8 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 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 Often it is only the damaged blank nut itself poorly shaped from overtightening that causes a failure of the test Before investigating on any other possible sources of failure make sure that the blank nut you are using is in good condition and properly tightened No pressure increase or minimum pressure of plateau 1 not reached Probable cause Suggested actions 1 Pump not running Check the logbook for error messages 2 Wrong solvent line connections to solvent Ensure the solvent lines from the degasser to selection valve the solvent selection valve are connected correctly 3 Loose or leaky fittings Ensure all fittings are tight or exchange capillary 4 La
4. 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 not secured or pump head not seated e g capillary is trapped between the pump correctly head and body 2 Broken piston Exchange the piston Index Limit Index Limit Pump channel A B Index Limit Pump channel B The time required by the piston to reach the encoder index position was too short pump 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 index position is reached too fast the error message is generated Probable cause Suggested actions 1 Irregular or sticking drive movement Remove the pump head and examine the seals pistons and internal components for signs of wear contamination or damage Exchange components as required 2 Defective pump drive assembly Please contact your Agilent service representative 1260 Capillary Pump User Manual 107 7 108 Error Information Index Adjustment Index Adjustment Pump channel A B Index Adjustment Pump channel B The encoder index po
5. gt In step 10 of following procedure use the PEEK blank nut from the accessories kit to block the flow sensor outlet 114 1 Select the Micro Mode Pressure Test from the test selection menu 2 Start the test and follow the instructions For detailed instructions refer to the Agilent Lab Advisor software 1260 Capillary Pump User Manual Test Functions and Calibration 8 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 1000 nL min 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 If the test fails again insert the blank nut at the outlet of the previous module in the stack and repeat the pressure test Exclude each module one by one to determine which module is leaky Potential Causes of Micro Mode Pressure Test Failure After isolating and fixing the cause of the leak repeat the pressure test to confirm the system is tight Table 22 Potential Cause Pump Potential Cause Pump Corrective Action Loose or leaky fitting Tighten the fitting or exchange the capillary High flow sensor offset Run the flow sensor accuracy calibration and correct the flow sensor offset Table 23 Potential Cause Autosampler Potential Cause
6. 3395A integrator see details in section Remote Cables on page 176 03396 61010 Agilent module to 3396 Series III 3395B integrators 5061 3378 Agilent module to Agilent 35900 A D converters or HP 1050 1046A 1049A 01046 60201 Agilent module to general purpose BCD cables p n Description 03396 60560 Agilent module to 3396 integrators G1351 81600 Agilent module to general purpose 1260 Capillary Pump User Manual Identifying Cables 11 CAN cables p n Description 5181 1516 CAN cable Agilent module to module 0 5 m 5181 1519 CAN cable Agilent module to module 1 m LAN cables p n Description 5023 0203 Cross over network cable shielded 3 m for point to point connection 5023 0202 Twisted pair network cable shielded 7 m for point to point connection External Contact Cable p n Description G1103 61611 External contact cable Agilent module interface board to general purposes RS 232 cables p n Description G1530 60600 RS 232 cable 2m RS232 61600 RS 232 cable 2 5m Instrument to PC 9 to 9 pin female This cable has special pin out and is not compatible with connecting printers and plotters It s also called Null Modem Cable with full handshaking where the wiring is made between pins 1 1 2 3 3 2 4 6 5 5 6 4 7 8 8 7 9 9 5181 1561 RS 232 cable 8m 1260 Capillary Pump User Manual 173 11 Identifying Cables Analog Cables 174 One end of these cables provides a BNC connect
7. Make sure the set solvent volume matches the actual bottle filling and set the shutoff limit to a reasonable value e g 100 mL for 1 L bottles The system pressure has exceeded the upper pressure limit Probable cause 1 Upper pressure limit set too low 2 Blockage in the flowpath after the damper 3 Defective damper 4 Defective main board 1260 Capillary Pump User Manual Suggested actions Ensure the upper pressure limit is set to a value suitable for the analysis Check for blockage in the flowpath The following components are particularly subject to blockage inline filter frit needle autosampler seat capillary autosampler sample loop autosampler column frits and capillaries with small internal diameters e g 50 um ID Please contact your Agilent service representative Please contact your Agilent service representative 97 7 98 Error Information Pressure Below Lower Limit The system pressure has fallen below the lower pressure limit Probable cause 1 2 Solvent bottle empty Lower pressure limit set too high Air bubbles in the mobile phase Leak Defective damper Defective main board Defective active inlet valve AIV Defective outlet ball valve OBV Suggested actions Replenish solvent Ensure the lower pressure limit is set to a value suitable for the analysis Ensure solvents are degassed Purge the module Ensure solvent inlet filters
8. Micro Mode Pressure Test 114 Running the Test from the Agilent Lab Advisor Software 114 Micro Mode Pressure Test Results 115 Normal Mode Pressure Test 116 Positioning the Blank Nut 117 Running the Pressure Test 118 Evaluating the Results 119 Leak Test 120 Leak Test Description 120 Running the Leak Test 122 Evaluating the Results 123 EMPV Test 127 EMPV Test Description 127 Running the EMPV Test 127 EMPV Cleaning 128 1260 Capillary Pump EMPV Cleaning Description 128 Running the Test 128 This chapter describes the tests for the module te Agilent Technologies 113 Test Functions and Calibration 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 Step 1 The test begins with the initialization of both pump heads Next pump A begins pumping solvent until a system pressure of 380 bar is reached Step 2 The pump is operating in the Pressure Control Mode at 380 bar for several minutes The remaining flow in the column flow path between the EMPV and the blank nut is measured Running the Test from the Agilent Lab Advisor Software CAUTION Stainless steel blank nuts can damage the flow sensor
9. Autosampler Corrective Action Loose or leaky fitting Tighten or exchange the fitting or capillary Needle seat Exchange the needle seat assembly Rotor seal injection valve Exchange the rotor seal Damaged metering seal or piston Exchange the metering seal Check the piston for scratches Exchange the piston if required 1260 Capillary Pump User Manual 115 Test Functions and Calibration Normal Mode Pressure Test 116 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 Preparation 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 Move the inline filter outlet capillary from the EMPV to the manual purge valve Step 1 The test begins with the initialization of both pumpheads After initialization pistons Al and B1 are both at the top of their stroke Next pump A begins pumping solvent with a flow rate of 510 uL min and stroke of 100 uL The pump continues to pump until a system pressure of 390 bar is reached For this test only channel A2 is active To test the pressure tightness of
10. Replace piston if scratched A SN Piston surface 1260 Capillary Pump User Manual 151 9 Maintenance Exchanging the Pistons 3 Reassemble the pump head assembly see Reassembling the Pump Head Assembly on page 154 152 1260 Capillary Pump User Manual Maintenance 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 60001 Flow sensor 20 pL 1260 Capillary Pump 1 G1376 60002 100ul 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 5 Using a 1 4 inch wrench reconnect the capillaries coming from the EMPV going to the injection device port 1 1260 Capillary Pump User Manual 153 9 Maintenance 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 installed and snap the pump head and piston housing together Pump head Piston housing 2 Tighten the lock screw Lock screw 154 1260 Capillary Pump User Manual Maintenance 9 Reassembling the Pump Head Assembly 3 Carefully insert the pis
11. full duplex 1 1 1 Xx x xX Bootp x xX x 0 0 0 Bootp amp Store Xx X X 0 0 1 Using Stored x X x 0 1 0 Using Default Xx xX xX 0 1 1 TEST 1 1 System NVRAM Boot Resident System 1 X Revert to Default Data Coldstart X X X 1 Legend 0 switch down 1 switch up x any position When selecting the mode TEST the LAN settings are Auto Negotiation amp Using Stored For explanation of Boot Resident System and Revert to Default Data Coldstart refer to Special Settings on page 30 26 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Capillary Pump 1 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 Figure 6 Configuration switch settings depend on configured mode All modules without on board LAN e default is ALL DIPS DOWN best settings Bootp mode for LAN e for boot test modes DIPS 1 2 must be UP plus required mode Switch settings provide configuration parameters for GPIB address serial communication protocol and instrument specific initialization procedures With the introduction of the Agilent 1260 Infinity all GPIB interfaces have been removed The preferred communication is LAN The following tables represent the configuration switch sett
12. internet 194 introduction to the pump 8 L LAN cable 181 leak sensor open 94 leak test evaluation 123 leak test 120 leak sensor short 94 leak 96 line frequency 37 line voltage 37 liquimeter 149 lithium batteries 190 M main assemblies parts 160 1260 Capillary Pump User Manual Index main assemblies overview 132 maintenance procedures 135 maintenance feedback 15 replacing firmware 15 7 157 message remote timeout 93 missing pressure reading 100 missing parts 42 motor drive power 103 non operating altitude 37 non operating temperature 37 0 operating Altitude 37 operating temperature 37 optimization stack configuration 44 outlet valve 132 142 overview pump 10 P packaging damaged 42 parts main assemblies 160 parts identification cables 171 parts accessory kit 43 169 bottle head assembly 163 damaged 42 flow sensor 168 hydraulic path 164 missing 42 pump head 166 pump housing 160 1260 Capillary Pump User Manual solvent cabinet 163 performance specification 38 pH range 38 physical specifications 37 piston 132 151 power supply indicator 84 power consideration 34 power consumption 37 power cords 35 power switch 50 pressure above upper limit 97 pressure below lower limit 98 pressure sensor readings 52 pressure pulsation 14 78 pressure range 75 pressure operating range 38 priming witha pump 59 PTFE frit 132 PTFE frit 144 PTFE lubricant 154 pump head assembly 166 pump h
13. o0 oo og 3 Gray Start Low KEY coal oo BG 4 Blue Shut down Low o0 am 5 Pink Not connected oOo 0 ji 6 Yellow Power on High O 7 Red Ready High 8 Green Stop Low 9 Black Start request Low 178 1260 Capillary Pump User Manual BCD Cables Identifying Cables 11 One end of these cables provides a 15 pin BCD connector to be connected to the Agilent modules The other end depends on the instrument to be connec ted to Agilent Module to General Purpose p n G1351 81600 Wire Color Pin Agilent Signal Name BCD Digit module Green 1 BCD 5 20 Violet 2 BCD7 80 4 Blue 3 BCD 6 40 m Yellow 4 BCD 4 10 SS Black 5 BCD 0 1 ay Orange 6 BCD 3 8 Red 7 BCD 2 4 Brown 8 BCD 1 2 Gray 9 Digital ground Gray Gray pink 10 BCD 11 800 Red blue 11 BCD 10 400 White green 12 BCD 9 200 Brown green 13 BCD 8 100 notconnected 14 notconnected 15 5V Low 1260 Capillary Pump User Ma 179 11 Identifying Cables Agilent Module to 3396 Integrators p n 03396 60560 Pin 3396 Pin Agilent Signal Name BCD Digit module 1 1 BCD 5 20 2 2 BCD7 80 8e 7 3 3 BCD6 40 4 4 BCD 4 10 5 5 BCDO 1 1e 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 5V Low 180 1260 Capillary Pump User Manual CAN LAN Cables Identifying Cables 11 Both ends of this cable provide a modular plug to be connected to Agilent modules CAN or LAN connectors CAN
14. 103 pressure above upper limit 97 pressure below lower limit 98 pump head missing 107 remote timeout 93 selection valve failed 99 selection valve fuse 101 servo restart failed 106 shut down 92 stroke length 109 synchronization lost 93 temperature limit exceeded 102 temperature out of range 102 timeout 92 error message wait timeout 110 error zero solvent counter 97 196 exchanging active inlet valve 139 active inlet valve 132 139 interface board 156 outlet valve sieve 132 142 outlet valve 132 142 pistons 132 151 pump seals 132 148 purge valve frit 132 144 purge valve 132 144 solvent selection valve 144 wash seals 132 153 153 external contact cable 182 F fan failed 96 features GLP 39 safety and maintenace 39 firmware updates 157 157 upgade downgrade 157 upgrade downgrade 157 flow sensor parts 168 flow connections 54 flow precision 38 flow range 38 frequency range 37 frit 144 G general error messages 92 hexagonal key 3mm 148 151 hexagonal key 3mm 146 154 hexagonal key 4mm 148 151 hexagonal key 4mm 146 154 hints for successful use 62 humidity 37 hydraulic path parts 164 hydraulic system 38 index limit 107 index adjustment 108 index missing 108 initialization failed 109 inlet valve fuse 101 inlet valve missing 104 installation pump module 49 installation bench space 36 instrument check 67 instrument layout 16 interface board 156 interface cable 51 interfaces 19
15. 61315 45003 61375 87310 8710 1534 8710 0806 2x G1376 90014 1260 Capillary Pump User Manual Description Mounting screw for manual purge valve holder M4 20 mm long Tubing Flexible 1 ea 1 meter Washer for purge valve holder screw Replacement SS frit 0 5 um pore size CAN cable Agilent module to module 1 m Insert tool Solvent inlet filter stainless steel Manual purge valve Holder for manual purge valve Torque adapter Fused silica PEEK capillary 50 pm55 cm 20 pL flow sensor Wrench 4 mm both ends open end Wrench open end 1 2 inch and 7 16 inch Agilent 1260 Infinity Capillary Pump User Manual 43 3 Installing the Module Optimizing the Stack Configuration 44 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 One Stack Configuration Ensure optimum performance by installing the modules of the Agilent 1260 Infinity LC System in the following configuration See Figure 7 on page 45 and Figure 8 on page 46 This configuration optimizes the flow path for minimum delay volume and minimizes the bench space required 1260 Capillary Pump User Manual Solvent cabinet Vacuum degasser Local User Interface Autosampler Column compartment Detector Installing the Module Optimizing
16. Cables p n 5181 1516 5181 1519 LAN Cables p n 5023 0203 5023 0202 1260 Capillary Pump User Manual Description CAN cable Agilent module to module 0 5 m CAN cable Agilent module to module 1 m Description Cross over network cable shielded 3 m for point to point connection Twisted pair network cable shielded 7 m for point to point connection 181 11 Identifying Cables External Contact Cable 5o C G 1 100 lt 6 ie e e11 One end of this cable provides a 15 pin plug to be connected to Agilent modules interface board The other end is for general purpose Agilent Module Interface Board to general purposes p n G1103 61611 Color Pin Agilent Signal Name module White 1 EXT 1 a Brown 2 EXT 1 x Green 3 EXT 2 Bea Yellow 4 EXT 2 Grey 5 EXT 3 Pink 6 EXT 3 Blue 7 EXT 4 Red 8 EXT 4 Black 9 Not connected Violet 10 Not connected Grey pink 11 Not connected Red blue 12 Not connected White green 13 Not connected Brown green 14 Not connected White yellow 15 Not connected 182 1260 Capillary Pump User Manual Identifying Cables 11 Agilent Module to PC p n Description G1530 60600 RS 232 cable 2m RS232 61600 RS 232 cable 2 5m 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
17. G1375 87301 Capillary EMPV to flow sensor 100 uL flow sensor p n G1375 87305 2 3 Capillary damper to mixer capillary pump only p n 01090 87308 4 Capillary filter to EMPV p n G1375 87400 5 Capillary flow sensor to injection device 20 pL 50 pm i d 55 cm length PEEK fused silica p n G1375 87310 Capillary flow sensor to injection device 100 pL flow sensor 100 pm ID x 55cm p n G1375 87306 6 Restriction capillary p n G1312 67304 7 Mixing capillary p n G1312 67302 8 Connecting tube SSV to AIV p n G1311 67304 9 Bottle head assembly p n G1311 60003 1260 Capillary Pump User Manual 57 3 Installing the Module 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 The pump should never be used for priming empty tubings never let the pump run dry Use the syringe to draw enough solvent for completely filling the tubings to the pump inlet before continuing to prime with the pump Manually Priming the Solvent Channels WARNING Liquid may drip from the disconnected solvent tube gt Make sure to follow appropriate safety precautions 58 This procedure should be carried out before the modules are turned on 1 The degasser accessory kit contains a 20 mL plastic syringe and a solvent tube adapter for the syringe P
18. Module to 3396 Series II 3395A Integrators Use the cable Agilent module to 3396A Series I integrators p n 03394 60600 and cut pin 5 on the integrator side Otherwise the integrator prints START not ready 1260 Capillary Pump User Manual Identifying Cables 11 Agilent Module to 3396 Series III 3395B Integrators p n 03396 61010 Pin 33XX Pin Agilent Signal Name Active module TTL 9 1 White Digital ground gt NC 2 Brown Prepare run Low e 3 3 Gray Start Low m s NC 4 Blue Shut down Low e O a NC 5 Pink Not connected NC 6 Yellow Power on High o 14 7 Red Ready High 4 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent Module to Agilent 35900 A D Converters p n 5061 3378 Pin 35900 A D Pin Agilent Signal Name Active module TTL 1 White 1 White Digital ground 2 Brown 2 Brown Prepare run Low 3 Gray 3 Gray Start Low 4 Blue 4 Blue Shut down Low 5 Pink 5 Pink Not connected 6 Yellow 6 Yellow Power on High 7 Red 7 Red Ready High 8 Green 8 Green Stop Low 9 Black 9 Black Start request Low 1260 Capillary Pump User Manual 177 11 Identifying Cables Agilent Module to General Purpose p n 01046 60201 Pin Universal Pin Agilent Signal Name Active module TTL 1 White Digital ground A O 1 2 B oo Brown Prepare run Low
19. actions 1 Defective or disconnected pump encoder Please contact your Agilent service connector representative 2 Defective pump drive assembly Please contact your Agilent service representative Inlet Valve Missing Inlet Valve Missing Pump channel A B Inlet Valve Missing Pump channel B The active inlet valve in the module is missing or defective The processor checks the presence of the active inlet valve connector every 2 seconds If the connector is not detected by the processor the error message is generated Probable cause Suggested actions 1 Disconnected or defective cable Please contact your Agilent service representative 2 Disconnected or defective connection cable Please contact your Agilent service front panel to main board representative 3 Defective active inlet valve Exchange the active inlet valve 104 1260 Capillary Pump User Manual Error Information 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 2 Defective flow sensor Please contact your Agilent service representative Leak Sensor Missing Probable c
20. and e output are open collector type inputs outputs wired or technique All common TTL circuits operate with a 5 V power supply A TTL signal is defined as low or L when between 0 V and 0 8 V and high or H when between 2 0 V and 5 0 V with respect to the ground terminal Table4 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 Receiver is any module capable to reduce safety risk 1260 Capillary Pump User Manual 23 1 24 Introduction to the 1260 Infinity Capillary Pump Table4 Remote Signal Distribution Pin Signal Description 5 Not used 6 POWER ON H All modules connected to system are switched on Receiver is any module relying on operation of others 7 READY H System is ready for next analysis Receiver is any sequence controller 8 STOP L Request to reach system ready state as soon as possible for example stop run abort or finish and stop injection Receiver is any module performing run time controlled activities 9 START REQUEST L Request to start injection cycle for example by start key on any module Receiver is the aut
21. 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 Temperature Limit Exceeded Temperature Limit Exceeded 0 Pump channel A Temperature Limit Exceeded 1 Pump channel B The temperature of one of the motor drive circuits is too high The processor continually monitors the temperature of the drive circuits on the main board If excessive current is being drawn for long periods the temperature of the circuits increases If the temperature exceeds the upper limit the error message is generated Probable cause Suggested actions 1 High friction partial mechanical blockage in Ensure the capillaries and frits between the the pump drive assembly pump head and damper inlet are free from blockage 2 Partial blockage of the flowpath in front of Ensure the outlet valve is not blocked the damper 3 Defective pump drive assembly Please contact your Agilent service representative 4 Defective main board Please contact your Agilent service representative 1260 Capillary Pump User Manual Error Information 7 Motor Drive Power Motor Drive Power Pump channel A B Motor Drive Power Pump channel B 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 re
22. cable 174 oe Ang vainly et ene 173 AUTO mode 14 LAN 173 AUX output 52 overview 172 remote 1 2 B RS 232 173 battery CAN safety information 190 cable 181 BCD board 156 check out sample 67 BCD cleaning 134 cable 179 Communication settings bench space 36 RS 232C 28 blockage 103 compensation sensor open 95 1260 Capillary Pump User Manual compensation sensor short 95 composition precision 38 composition range 38 compressibility compensation 38 78 condensation 36 configuration one stack 44 44 two stack 47 connections flow 54 connect vacuum degasser 52 control software 53 counter seal wear 135 counter EMF 135 D damaged parts 42 defect on arrival 42 delay volume 38 delivery checklist 42 Diagnostic software 87 dimensions 37 disassembling the pump head 146 E early maintenance feedback 135 electrical connections descriptions of 17 electronic waste 189 electrostatic discharge ESD 156 EMF flag 135 EMF counters 135 EMF limits 136 195 Index EMF early maintenance feedback 15 EMPV cleaning procedure 128 EMPV test 127 EMPV cleaning 83 encoder missing 104 error messages fan failed 96 error messages compensation sensor open 95 compensation sensor short 95 encoder missing 104 index adjustment 108 index limit 107 index missing 108 initialization failed 109 inlet valve fuse 101 inlet valve missing 104 eak sensor open 94 eak sensor short 94 eak 96 missing pressure reading 100 motor drive power
23. exchanged The test should also be done if column flow stability problems occur micro mode only The EMPYV 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 The test starts with a short flushing sequence and a cleaning procedure for the EMPV Afterwards low and high pressure is controlled by the EMPV and the appropriate current is monitored Finally a linear pressure ramp is performed Running the EMPV Test 1 Fill vacuum degasser with A1 aqueous solvent B1 organic solvent acetonitrile methanol isopropanol etc 2 If vacuum degasser is totally empty use syringe to draw solvent into the vacuum chamber or flush vacuum degasser before test is executed test requires filled degasser chambers 3 Plug the pump outlet with blank nut at EMPV outlet 4 Disconnect the EMPV to flow sensor capillary G1375 87301 at EMPV outlet and plug the EMPV outlet port with blank nut 01080 83202 5 Execute test 6 Remove the blank nut 7 Reconnect the EMPV to flow sensor capillary Do not overtighten 1260 Capillary Pump User Manual 127 8 Test Functions and Calibration EMPV Cleaning 1260 Capillary 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 t
24. following to occur Increased system pressure caused by clogging of the inline filter Algae deposits are barely visible on the stainless steel filter frit Replace the frit if the backpressure of the pump in purge mode water 2 5 mL min exceeds 20 bar e Short lifetime of solvent filters bottle head assembly A blocked solvent filter in the bottle especially when only partly blocked is more difficult to identify and may show up as gradient performance problems intermittent pressure fluctuations etc 1260 Capillary Pump User Manual 65 4 Using the Pump 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 e Always use freshly prepared solvents especially use demineralized water which was filtered through about 0 2 um filters e Never leave mobile phase in the instrument for several days without flow e Always discard old mobile phase e Use the amber solvent bottle Solvent bottle amber p n 9301 1450 supplied with the instrument for your aqueous mobile phase e If possible add a few mg l sodium azide or a few percent organic solvent to the aqueous mobile phase 66 1260 Capillary Pump User Manual Inject the Check out Sample Using the Pump 4 The purpose of the instrument check is to demonstrate that all modules of the instrument are correctly installed and connected It is not a test of the instrumen
25. gt Never use the module without solvent inlet filter The solvent filters are located on the low pressure side of the pump A blocked filter therefore does not affect the pressure readings of the pump The pressure readings cannot be used to check whether the filter is blocked or not If the filter is in good condition the solvent will freely drip out of the solvent tube due to hydrostatic pressure If the solvent filter is partly blocked only very little solvent will drip out of the solvent tube 1260 Capillary Pump User Manual 137 9 Maintenance 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 138 1260 Capillary Pump User Manual Maintenance 9 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 Tools required Wrench 14 mm Parts required p n Description 1 G1312 60025 Active inlet valve body optional without cartridge 1 5062 8562 Active Inlet Valve Cartridge 400 bar 1 G1311 67304 Connecting tube MCGV to AIV Unplug the active inlet valve cable from the connector 2 Disconnect the solvent inlet tube at the inlet valve bewa
26. of the hazard involved Do not attempt internal service or adjustment unless another person capable of rendering first aid and resuscitation is present Do not replace components with power cable connected Do not operate the instrument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or make any unauthorized modification to the instrument Capacitors inside the instrument may still be charged even though the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious personal injury are present in this instrument Use extreme caution when handling testing and adjusting When working with solvents please observe appropriate safety procedures e g goggles safety gloves and protective clothing as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used 1260 Capillary Pump User Manual 187 12 Appendix Safety Symbols Table 25 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the A 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
27. short time The fast gradient range This range is recommended for running fast gradient e g lt 3 min The equilibration time is optimized The primary flow is strongly dependant on the system pressure and internal volume of the flow path of the pump which is defined by the type of inline filter the presence or absence of the static mixer and the flow sensor configuration Table 19 on page 76 gives approximate primary flow values in function of the system pressure and the set primary flow range Table 19 Primary flow overview for standard pump configuration 0 bar 100 bar 200 bar 300 bar 400 bar System System System System System pressure pressure pressure pressure pressure Low consumption range 200 225 250 275 300 Default range 500 570 640 710 780 Fast gradient range 800 995 1190 1385 1580 In any case the standard configuration is changed the primary flow could be higher compared to the values in above table 76 1260 Capillary Pump User Manual Optimizing Performance 5 Static Mixer and Filter Static Mixer and Filter The 1260 Capillary Pump is equipped with a static mixer and an inline filter in front of the EMPV The Standard Static Mixer The standard static mixer has a volume of typically 420 uL In order to reduce the delay volume of the 1260 Capillary Pump you can remove the mixer Conditions to remove the static mixer e The delay volume of the pump should be reduced to a minimum for fastest gradient r
28. the Stack Figure 7 Recommended Stack Configuration for 1260 Front View 1260 Capillary Pump User Manual Configuration 3 45 3 Installing the Module Optimizing the Stack Configuration Remote cable CAN Bus cable to local user interface CAN Bus cable Analog detector signal 1 or 2 outputs per detector AC power LAN to LC ChemStation location depends on detector Figure 8 Recommended Stack Configuration for 1260 Rear View 46 1260 Capillary Pump User Manual Installing the Module 3 ng the lt Configuratio 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 9 on page 47 and Figure 10 on page 48 Instant Pilot Detector Column compartment Autosampl
29. to fix the problem are provided see chapter Error Information Test Functions A series of test functions are available for troubleshooting and operational verification after exchanging internal components see Tests and Calibrations System Pressure Test The System Pressure Test is a quick test designed to determine the pressure tightness of the system After exchanging flow path components e g pump seals or injection seal use this test to verify the system is pressure tight 82 1260 Capillary Pump User Manual Troubleshooting and Diagnostics 6 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 EMPV Cleaning The pump is equipped with a 0 5 um pore width inline filter Although it retains most particles particular matter will over time collect in the EMPV electromagnetic proportioning valve causing unstable micro flow and pressure The EMPV cleaning procedure quickly and reliably removes these particles to restore pump performance in micro mode 1260 Capillary Pump User Manual 83 6 Troubleshooting and Diagnostics Status Indicators Two status indicators are lo
30. uL Injection mode Edit inj prog Inject Bypass Verify that the injection valve is set to Mainpass in the Set Injection Valve box of the Autosampler Configuration dialog 1260 Capillary Pump User Manual 71 4 72 Using the Pump 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 um 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 Due to capillary ID tolerances the nominal pressure at 600 nL min and 300 nL min might be different from system to system These differences can be up to 40 The evaluation is done by a visual inspection of the test results The average pressure between the different plateaus at the same flow rate must be ina range of 2 bar and typically 1 The pressure at 300 nL min should be half of the pressure at 600 nL min If no UV detector is connected to the system you will not be able to open your test data file to review the pressure and the flow profile acquired during the run In this case locate and copy the signal file DAD1A CH from the directory HHCHEM 1 DATA DEMO ISOCRA D to the directory for your checkout test data file before opening the file for review If the test results are not in the expected range verify that the flow path has been thoroughly flushed and is filled
31. 0 6 bar Acetone 126 Acetonitrile 115 Benzene 95 Carbon tetrachloride 110 Chloroform 100 Cyclohexane 118 Ethanol 114 Ethyl acetate 104 Heptane 120 Hexane 150 Isobutanol 100 Isopropanol 100 Methanol 120 i Propanol 100 Toluene 87 THF 95 Water 46 1260 Capillary Pump User Manual 79 5 Optimizing Performance How to Optimize the Compressibility Compensation Setting 80 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual 6 Troubleshooting and Diagnostics Overview of the Module s Indicators and Test Functions 82 Status Indicators 84 Power Supply Indicator 84 Module Status Indicator 85 User Interfaces 86 Agilent Lab Advisor Software 87 This chapter provides information about the module s status indicators error messages and the available test functions in Instant Pilot and Lab Advisor ee Agilent Technologies 81 6 Troubleshooting and Diagnostics 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 Error Messages In the event of an electronic mechanical or hydraulic failure the module generates an error message in the user interface For each message a short description of the failure a list of probable causes of the problem and a list of suggested actions
32. 164 Description Bottle head assembly Connecting tube SSV to AIV Capillary outlet valve to piston 2 Restriction capillary Mixing capillary Capillary damper to mixer capillary pump only Mixer capillary pump only Capillary mixer to filter capillary pump only Filter assembly includes frit Replacement SS frit 0 5 um pore size Capillary filter to EMPV Capillary EMPV to flow sensor 20 uL flow sensor Capillary EMPV to flow sensor 100 uL flow sensor Capillary flow sensor to injection device 20 uL 50 pm i d 55 cm length PEEK fused silica Capillary flow sensor to injection device 100 uL flow sensor 100 um ID x 55 cm Corrugated waste tubing 5 m reorder pack 1260 Capillary Pump User Manual Parts and Materials for Maintenance 10 Hydraulic Path 7 6 11 J ZA K g gt 12 10 ANES Sy JA N ANS hs ae i Crea EF AKAN N Gf R Q CS 5 dh D Q IDA S BSN ES D Y lt Doo onono 9 2 Figure 27 Hydraulic Path 1260 Capillary Pump User Manual 165 10 Parts and Materials for Maintenance Pump Head Assembly Item p n G1312 60064 1 5067 4695 G1312 60062 3 G4220 63015 G4220 24013 4 5063 6589 0905 1420 5 G1312 67300 6 G1312 25260 7 G1312 60025 5062 8562 8 G1312 60067 9 5042 1303 10 G1312 23201 11 0515 2118 Description Pump Head without Seal Wash Sapphire piston default Adapter integrated 1260 Support Ring without Seal Wash Backup Ring for Seal Holde
33. 315C D DAD and G1365C D MWD This interface allows the control of the module system via a connected PC with the appropriate control software If an Agilent detector DAD MWD FLD VWD RID is in the system the LAN should be connected to the DAD MWD FLD VWD RID due to higher data load If no Agilent detector is part of the system the LAN interface should be installed in the pump or autosampler RS 232C Serial The RS 232C connector is used to control the module from a computer through RS 232C connection using the appropriate software This connector can be configured with the configuration switch module at the rear of the module Refer to Communication Settings for RS 232C There is no configuration possible on main boards with on board LAN These are pre configured for e 19200 baud e 8 data bit with no parity and one start bit and one stop bit are always used not selectable 1260 Capillary Pump User Manual 21 1 22 Introduction to the 1260 Infinity Capillary Pump The RS 232C is designed as DCE data communication equipment with a 9 pin male SUB D type connector The pins are defined as Table 3 RS 232C Connection Table Pin Direction Function 1 In DCD 2 In RxD 3 Out TxD 4 Out DTR 5 Ground 6 In DSR 7 Out RTS 8 In CTS 9 In RI Instrument PC DCD 1 1 DCD RX 2 a7 2 RX TX 3 X 3 TX DTR 4 4 DTR GND 5 y 5 GND DSR 6 6 DSR RTS 7 3 7 RTS CTS 8 X 8 CTS RI 9 9 RI DB9 DB9 DB9
34. 4 7 8 8 7 9 9 5181 1561 RS 232 cable 8m 1260 Capillary Pump User Manual 183 11 Identifying Cables Agilent 1200 Module to Printer p n Description 5181 1529 Cable Printer Serial amp 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 184 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual 12 Appendix General Safety Information 186 The Waste Electrical and Electronic Equipment Directive 189 Batteries Information 190 Radio Interference 191 Sound Emission 192 Solvent Information 193 Agilent Technologies on Internet 194 This chapter provides addition information on safety legal and web ee Agilent Technologies 185 12 Appendix 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 Ensure the proper usage of the equipment The protection provided by the equipment may be impaired gt The operator of this instrument is advised to use the equipment in a manner as specified in this manual Safety Standards This is a Safety Cla
35. 60 Capillary Pump User Manual 10 Parts and Materials for Maintenance Pump Housing and Main Assemblies 160 Solvent Cabinet and Bottle Head Assembly 163 Hydraulic Path 164 Pump Head Assembly 166 Flow Sensor Assembly 168 Capillary Pump Accessory Kit 169 This chapter provides information on parts for maintenance ee Agilent Technologies 159 10 Parts and Materials for Maintenance 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 G1376 65030 Capillary system main board CSM G1376 69030 Exchange assembly CSM board 5 G4280 81618 Cable assembly solvent selection valve G1312 05208 SSV holder G1312 05207 Holder for SSV connector 6 3160 1017 Fan assembly 7 79835 60005 Damper 8 G4280 60028 Solvent selection valve 5022 2112 Screw for cover and Z panel 9 5042 8590 Leak plane 10 G1361 60000 EMPV assembly 11 G1376 60001 Flow sensor 20 uL 1260 Capillary Pump 11 G1376 60002 Flow sensor 100 pL 1260 Capillary Pump 160 1260 Capillary Pump User Manual Parts and Materials for Maintenance 10 Pump Housing and Main Assemblies Cee Ova Ol fee NI A 4 Ts TH S tie Figure 24 Overview of Main Assemblies Front View 1260 Capillary Pump User Manual 161 10 Pa
36. 800 1 1 1 38400 Table9 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 Switches Parity 7 8 0 0 No Parity 1 0 Odd Parity 1 1 Even Parity One start bit and one stop bit are always used not selectable Per default the module will turn into 19200 baud 8 data bit with no parity 1260 Capillary Pump User Manual 29 1 Introduction to the 1260 Infinity Capillary Pump Special Settings The special settings are required for specific actions normally in a service case 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 If you use the following switch settings and power the instrument up again the instrument firmware stays in the resident mode It is not operable as a module It only uses basic functions of the operating system for example for communication In this mode the main firmware can be loaded using update utilities Table 11 Boot Resident Settings without on board LAN Mode Select SW1 sw2 SW3 Sw4 SW5 SW6 Sw7 Swe LAN TEST BOOT 1 1 1 0 0 0 0 0 No LAN TEST BOOT 1 1 0 0 1 0 0 0 30 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Cap
37. 9B Micro Degasser User Manual p n G1379 90013 74 1260 Capillary Pump User Manual Optimizing Performance 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 For applications that use normal phase solvents for example hexane we recommend using polyethylene pump seals PE seals pack of 2 p n 0905 1420 and Wash Seal PE p n 0905 1718 These seals have less abrasion compared to the standard seals Polyethylene seals have a limited pressure range of 0 200 bar When used above 200 bar their lifetime is reduced significantly DO NOT apply the seal wear in procedure performed with new standard seals at 400 bar 1260 Capillary Pump User Manual 75 5 Optimizing Performance How to Choose the Primary Flow The primary flow can be set in three ranges e 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 During step gradients at the end of the run the flow control may start to oscillate for a
38. AN Bus Power Plug Security Lever Figure 12 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 NOTE The power switch stays pressed in and a green indicator lamp in the power switch is on when the module is turned on When the line power switch stands out and the green light is off the module is turned off 8 Purge the pump see Priming Your System With the Pump on page 59 NOTE The pump shipps with default configuration settings To change these settings see Setting the 8 bit Configuration Switch without On Board LAN on page 27 1260 Capillary Pump User Manual 51 3 Installing the Module Connecting Modules and Control Software WARNING Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury gt Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Connecting Modules 1 Place the individual modules in a stack configuration as shown in Figure 7 on page 45 2 Ensure the power switches on the front of the modules are OFF switches stand out 3 Plug a CAN cable into the CAN connector at the rear of the respective module except vacuum degasser 4 Connect the CAN cable to the CAN connector of th
39. CAUTION Damage of the pump drive Starting the pump when the pump head is removed may damage the pump drive gt Never start the pump when the pump head is removed 1 Disconnect the capillary at the pumphead adapter and the tube at the active inlet valve Beware of leaking solvents Disconnect the active inlet valve cable plug AN Active inlet valve to mixer Plug Pumphead screws 2 Using a 4 mm hexagonal key step wise loosen and remove the two pump head screws and remove the pump head from the pump drive 146 1260 Capillary Pump User Manual Maintenance 9 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 Pump head Lock screw 4 Remove the support rings from the piston housing and lift the housing away from the pistons SSS gt Piston housing a Piston 1260 Capillary Pump User Manual 147 9 Maintenance Exchanging the Pump Seals and Seal Wear in Procedure When Tools required 3 mm hexagonal key 4 mm hexagonal key 1 4 inch wrench Parts required p n 2 5063 6589 standard or 0905 1420 for normal phase application 1 5022 2159 Description Seals pack of 2 Restriction capillary Seals leaking if indicated by the results of the pump test check both pump heads individually 1 Di
40. DB9 Male Female Female Male Figure 4 RS 232 Cable Analog Signal Output The analog signal output can be distributed to a recording device For details refer to the description of the module s main board 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Capillary Pump 1 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 The module provides one remote connector which is inputs outputs wired or technique To provide maximum safety within a distributed analysis system one line is dedicated to SHUT DOWN the system s critical parts in case any module detects a serious problem To detect whether all participating modules are switched on or properly powered one line is defined to summarize the POWER ON state of all connected modules Control of analysis is maintained by signal readiness READY for next analysis followed by START of run and optional STOP of run triggered on the respective lines In addition PREPARE and START REQUEST may be issued The signal levels are defined as e standard TTL levels 0 V is logic true 5 0 V is false e fan out is 10 e input load is 2 2 kOhm against 5 0 V
41. Exchanging the Pump Seals and Seal Wear in Procedure on page 148 Exchanging the Pistons on page 151 Exchanging the Flow Sensor on page 153 If internally leaking If internally leaking Unstable column flow or system pressure Column flow and system pressure drops from time to time If pump performance indicates seal wear If scratched Extended flow range 100 ul needed Leak on the flow sensor Unstable column flow Flow sensor blocked Pressure ripple unstable run leak test for verification Pressure ripple unstable run leak test for verification A pressure drop of gt 10 bar across the frit 2 5 mL min H20 with purge open indicates blockage Leaks at lower pump head side unstable retention times pressure ripple unstable run leak test for verification Seal life time shorter than normally expected check pistons while changing the seals Figure 17 on page 133 shows the main assemblies of the pump The pump heads and its parts do require normal maintenance for example seal exchange and can be accessed from the front simple repairs Replacing internal parts will require to remove the module from its stack and to open the top cover 132 1260 Capillary Pump User Manual Maintenance 9 Overview of Maintenance 5 6 7 4 3 8 9 10 2 12 Figure 17 Overview of Repair Procedures 12 Active inlet valve see Removing the Active Inlet Valve on page 139 23
42. Exchanging the Valve Cartridge 140 Replacing the Active Inlet Valve Body 140 Exchanging the Outlet Valve Sieve 142 Exchanging the Solvent Selection Valve 144 Removing and Disassembling the Pump Head 146 Exchanging the Pump Seals and Seal Wear in Procedure 148 Seal Wear in Procedure 150 Exchanging the Pistons 151 Exchanging the Flow Sensor 153 Reassembling the Pump Head Assembly 154 Exchanging the Optional Interface Board 156 Replacing Module Firmware 157 This chapter describes the maintenance of the module ot Agilent Technologies 129 9 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 24 on page 132 130 1260 Capillary Pump User Manual Maintenance 9 Warnings and Cautions WARNING Toxic flammable and hazardous solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks gt When working with these substances observe appropriate safety procedures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice gt The amount of substances should be reduced to the minimal volume required for the analysis gt Do not operate the ins
43. Notify your Agilent sales and service office about the damage gt An Agilent service representative will inspect the instrument at your site and initiate appropriate actions Delivery Checklist 42 Ensure all parts and materials have been delivered with the capillary pump The delivery checklist is shown in Table 15 on page 42 To aid in parts identification please see Parts and Materials for Maintenance on page 159 Please report missing or damaged parts to your local Agilent Technologies sales and service office Table 15 Capillary Pump Checklist Description Quantity Agilent 1260 Infinity Capillary Pump p n G1376 64050 1 Solvent cabinet including all plastic parts p n 5065 9981 1 Solvent bottle amber p n 9301 1450 1 Solvent bottle transparent p n 9301 1420 3 Analytical head assembly p n G1367 60003 4 Capillary flow sensor to injection device 20 pL 50 um i d 55 cm 1 length PEEK fused silica p n G1375 87310 Power cord 1 1260 Capillary Pump User Manual Installing the Module 3 Table 15 Capillary Pump Checklist Description Quantity CAN cable Agilent module to module 1 m p n 5181 1519 1 Remote cable As ordered Signal cable As ordered Service Manual 1 Accessory Kit p n G1376 68755 1 Capillary Pump Accessory Kit Accessory Kit p n G1376 68755 p n 0515 0175 0890 1760 2x 2190 0586 5022 2185 5181 1519 01018 23702 01018 60025 4x 61311 60009 61312 23200
44. Outlet ball valve see Exchanging the Outlet Valve Sieve on page 142 312 Solvent selection valve see Exchanging the Solvent Selection Valve on page 144 1260 Capillary Pump User Manual 133 9 Maintenance 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 WARNING Liquid dripping into the electronic compartment of your module Liquid in the module electronics can cause shock hazard and damage the module gt Do not use an excessively damp cloth during cleaning gt Drain all solvent lines before opening any fittings 134 1260 Capillary Pump User Manual Maintenance 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 The early maintenance feedback EMF feature monitors the usage of specific components in the instrument and provides feedback when the user settable limits have been exceeded The visual feedback in the user interface provides an indication that maintenance procedures should be scheduled EMF Counters The pump provides a
45. Pump 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 This pack is then housed in a metal inner cabinet which is enclosed by a plastic external cabinet The advantages of this packaging technology are e virtual elimination of fixing screws bolts or ties reducing the number of components and increasing the speed of assembly disassembly e the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations e the plastic layers help cushion the electronic and mechanical parts from physical shock and e the metal inner cabinet shields the internal electronics from electromagnetic interference and also helps to reduce or eliminate radio frequency emissions from the instrument itself 16 1260 Capillary Pump User Manual Electrical Connections Introduction to the 1260 Infinity Capillary Pump 1 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 e One analog output provides signals for integrators or data handling systems The interface board slot is
46. Typical Chromatogram A typical chromatogram for this analysis is shown in Figure 15 on page 68 The exact profile of the chromatogram will depend on the chromatographic conditions Variations in solvent quality column packing standard concentration and column temperature will all have a potential effect on peak retention and response Figure 15 Chromatogram 68 1260 Capillary Pump User Manual Using the Pump 4 Checkout procedure for a G2229A Nano LC System Parts required Preparations Use this procedure to confirm that the system has been installed correctly e the Nanoflow LC System performs within specification a technical problem is caused by the Nanoflow LC System Description G1379B 1260 Micro Degasser G2226A 1260 Nanoflow Pump G1377A 1260 Micro High Performance Autosampler G2226 67300 Nanoflow restriction capillary Channel A1 Water Channel B1 Acetonitrile Channel A2 Isopropanol 1 Purge channel Al with 100 water at 2 5 mL min for 2 min 2 Purge channel B1 with 100 aetonitrile at 2 5 mL min for 2 min You can speed up the preparation by skipping steps 3 and 4 and running step 7 in pressure control mode at 140 bar pressure control mode can be enabled in the module service center of Lab Advisor software 3 Pump 10 uL min normal mode 100 water for at least 5 min 4 Pump 10 uL min normal mode 100 B acetonitrile for at least 5 min Check the pressure tightness of the system by executing a m
47. alve EMPV Missing 105 App Agilent Technologies 89 7 90 Error Information Flow Sensor Missing 105 Leak Sensor Missing 105 Servo Restart Failed 106 Pump Head Missing 107 Index Limit 107 Index Adjustment 108 Index Missing 108 Stroke Length 109 Initialization Failed 109 Wait Timeout 110 Electronic fuse of SSV 111 This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions 1260 Capillary Pump User Manual Error Information 7 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 1260 Capillary Pump User Manual 91 7 Error Information General Error Messages 92 General error messages are generic to all Agilent series HPLC modules and may show up on other modules as well The timeout threshold was exceeded Probable cause 1 The analysis was completed successfully and the timeout function switched off the module as requested 2 Anot ready condition was present during a sequence or multiple injection run for a period longer than the timeout th
48. ance Specification Agilent 1260 Infinity Capillary Pump G1376A Type Specification Hydraulic system Settable column flow range Recommended column flow range Column flow precision Optimum composition range Composition precision Delay volume Pressure range Compressibility compensation Recommended pH range Two independent pump channels each with two pistons in series One proprietary servo controlled variable stroke drive per channel Floating pistons active inlet valves solvent selection valves two solvents per pump channel electronic flow control for flow rates up to 100 pL min 0 01 20 pL min 0 01 100 pL min with the extended flow range kit 0 001 2 5 pL min with the electronic flow control bypassed 1 20 pL min 10 100 pL min with extended flow range kit 0 1 2 5 mL min with the electronic flow sensor bypassed lt 0 7 RSD or 0 03 SD typically 0 4 RSD or 0 02 SD at 10 pL min and 50 pL min column flow based on RT default setting 1 99 or 5 pL min per channel primary flow whatever is greater lt 0 2 SD at 10 pL min 20 pL flow sensor 50 pL min 100 uL flow sensor minimum primary flow pump channel is 5 pL min primary flow 500 800 pL min Typically 3 uL from the electronic flow control to the pump outlet for flow rates up to 20 pL min Typically 12 uL from the electronic flow control to the pump outlet for flow rates up to 100 pL min For flow
49. and the cycle is repeated To mixing chamber From solvent bottle aE Oa Ball screw drive Motor with encoder Figure 2 Operating Principle of the Pump Head 12 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Capillary Pump 1 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 How Does Compressibility Compensation Work The compressibility of the solvents in use will affect retention time stability when the back pressure in the system changes for example aging of column In order to minimize this effect the pump provides a compressibility compensation feature which optimizes the flow stability according to the solvent type The compressibility compensation is set to a default value for each pump head independently The compensation value for each pump head can be changed through the user interface Without a compressibility compensation the following will happen during a stroke of the first piston The pressure in the piston chamber increases and the volume in the chamber will be compressed depending on backpressure and solvent type T
50. annels 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 2 Defective connection cable front panel to Please contact your Agilent service main board representative 3 Defective main board Please contact your Agilent service representative 4 1200 Series solvent selection valve installed Replace by 1260 solvent selection valve Inlet Valve Fuse Inlet Valve Fuse 0 Pump channel A Inlet Valve Fuse 1 Pump channel B One of the active inlet valves in the module has drawn excessive current causing the inlet valve electronic fuse to open Probable cause Suggested actions 1 Defective active inlet valve Restart the module If the error message appears again exchange the active inlet valve 2 Defective connection cable front panel to Please contact your Agilent service main board representative 3 Defective main board Please contact your Agilent service representative 1260 Capillary Pump User Manual 101 7 102 Error Information 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
51. apillary Pump User Manual Contents Static Mixer and Filter 77 How to Optimize the Compressibility Compensation Setting 78 Troubleshooting and Diagnostics 81 Overview of the Module s Indicators and Test Functions 82 Status Indicators 84 User Interfaces 86 Agilent Lab Advisor Software 87 Error Information 89 What Are Error Messages 91 General Error Messages 92 Module Error Messages 97 Test Functions and Calibration 113 Micro Mode Pressure Test 114 Normal Mode Pressure Test 116 Leak Test 120 EMPV Test 127 EMPV Cleaning 128 Maintenance 129 Introduction to Maintenance 130 Warnings and Cautions 131 Overview of Maintenance 132 Cleaning the Module 134 Early Maintenance Feedback EMF 135 Checking and Cleaning the Solvent Inlet Filters 137 Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve 139 Exchanging the Outlet Valve Sieve 142 Exchanging the Solvent Selection Valve 144 Removing and Disassembling the Pump Head 146 Exchanging the Pump Seals and Seal Wear in Procedure 148 Exchanging the Pistons 151 Exchanging the Flow Sensor 153 Reassembling the Pump Head Assembly 154 Exchanging the Optional Interface Board 156 Replacing Module Firmware 157 1260 Capillary Pump User Manual Contents 10 Parts and Materials for Maintenance 159 Pump Housing and Main Assemblies 160 Solvent Cabinet and Bottle Head Assembly 163 Hydraulic Path 164 Pump Head Assembly 166 Flow Sensor Assembly 168 Capil
52. apillary Pump User Manual 9 1 10 Introduction to the 1260 Infinity Capillary Pump Hydraulic Path Overview The capillary pump is based on the 1200 Series Binary Pump pressure limit 400 bar active inlet valves and performs all the functions necessary for a u flow solvent delivery system Basically these functions are e Low pressure metering and high pressure delivery e Solvent compressibility compensation e Variable stroke volume Column flow measurement and control Low pressure solvent metering and high pressure solvent delivery are accomplished by two pump channels each capable of delivering a maximum of 2 5 mL min flow at up to 400 bar pressure Each channel consists of an identical independently controlled pump unit Each pump unit includes a metering drive assembly and pump head assembly The pumphead assemblies both consist of two identical chambers pistons and seals plus an active inlet valve and an outlet valve The channel flow outputs are initially joined by a low volume pre mixer and are then connected by a capillary coil to a pressure pulse damper The pressure pulse damper also serves as a pressure transducer which sends system pressure information to the user interface In the capillary pump the flow output of the pressure pulse damper is connected to a mixer The standard mixer is a stainless steel tube filled with stainless steel balls The mixer is where most of the mobile phase mixing is accomplishe
53. are not blocked Inspect the pump head capillaries and fittings for signs of a leak Purge the module Run a pressure test to determine whether the seals or other module components are defective Please contact your Agilent service representative Please contact your Agilent service representative Replace AIV cartridge Replace OBV 1260 Capillary Pump User Manual Pressure Signal Missing Error Information 7 The pressure signal of the damper is missing The pressure signal of the damper must be within a specific voltage range If the pressure signal is missing the processor detects a voltage of approximately 120mV across the damper connector Probable cause 1 Damper disconnected 2 Defective damper Valve Failed Valve 0 Failed valve A1 Valve 1 Failed valve A2 Valve 2 Failed valve B2 Valve 3 Failed valve B1 Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative 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 1 Solvent selection valve disconnected 2 Connection cable inside instrument not connected 3 Connection cable inside instrument defective 4 Solvent selection valve defective 1260 Capillary Pump Us
54. ate 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 Al or channel A2 The pumphead B output may originate from either channel B1 or channel B2 In order to deliver fast gradients over the whole composition range the two pumpheads deliver a primary flow of 200 1100 uL min from which a mass flow sensor controlled electromagnetic proportioning valve EMPV splits the set column flow Excessive solvent is diverted to waste This electronic flow control automatically compensates for changes in solvent properties and backpressure throughout a run Solvent degassing is not done directly in the pump A 4 channel low volume micro vacuum degasser available as a separate module provides degassed solvents to the pump channel inputs Solvent degassing is required for best flow stability and detector stability especially at the low flow rates required to run capillary nano LC applications 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Capillary Pump 1 Introduction to the Pump Power supply CSM board Pump drive Damper Mixer Outlet valve Pump head A Flow sensor Active inlet valve Pump head B Leak sensor not installed Solvent selection valve Figure 1 Overview of the Pump 1260 C
55. ause Suggested actions 1 Disconnected or defective cable Please contact your Agilent service representative 2 Defective flow sensor Please contact your Agilent service representative 1260 Capillary Pump User Manual 105 7 Error Information Servo Restart Failed Servo Restart Failed Pump channel A B Servo Restart Failed Pump channel B 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 If the rotor is unable to move or if the C position cannot be reached the error message is generated Probable cause Suggested actions 1 Disconnected or defective cable Please contact your Agilent service representative 2 Mechanical blockage of the module Remove the pump head assembly Ensure there is no mechanical blockage of the pump head assembly or pump drive assembly 3 Defective pump drive assembly Please contact your Agilent service representative 4 Defective main board Please contact your Agilent service representative 106 1260 Capillary Pump User Manual Error Information 7 Pump Head Missing Pump Head Missing Pump channel A B Pump Head Missing Pump channel B The pump head end stop in the pump was not found
56. bles to the board connector BCD Interface board Figure 23 Exchanging the Interface Board 156 1260 Capillary Pump User Manual Maintenance 9 Replacing Module Firmware When Tools required Parts required Preparations 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 LAN RS 232 Firmware Update Tool or Agilent Diagnostic Software e Instant Pilot G4208A only if supported by module Description 1 Firmware tools and documentation from Agilent web site Read update documentation provided with the Firmware Update Tool To upgrade downgrade the module s firmware carry out the following steps 1 Download the required module firmware the latest LAN RS 232 FW Update Tool and the documentation from the Agilent web http www chem agilent com scripts cag_firmware asp 2 To load the firmware into the module follow the instructions in the documentation Module Specific Information There is no specific information for this module 1260 Capillary Pump User Manual 157 9 Maintenance Replacing Module Firmware 158 1260 Capillary Pump User Manual 12
57. bottle 2 If an AIV is installed screw the Adapter AIV to solvent inlet tubes p n 0100 1847 to the AIV and connect the inlet tube from the bottle head directly to it 3 Connect the restriction capillary 5022 2159 to the outlet of the EMPV Insert its other end into a waste container 4 Turn the system in purge mode and purge the system for 2 minutes with isopropanol at a flow rate of 2 ml min 5 Turn the system to Standard Mode set the flow to a rate adequate to achieve a pressure of 350 bar Pump 15 min at this pressure to wear in the seals The pressure can be monitored at your analog output signal with the Instant Pilot data system or any other controlling device connected to your pump 6 Turn OFF the pump slowly disconnect the restriction capillary from the EMPYV to release the pressure from the system Reconnect the capillary going to the flow sensor and the connecting tube from solvent selection valve to the AIV 7 Rinse your system with the solvent used for your next application 150 1260 Capillary Pump User Manual Exchanging the Pistons When When scratched Tools required 3 mm hexagonal key 4 mm hexagonal key p n 1 5063 6586 Parts required Description Piston Maintenance 9 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
58. cated on the front of the module The lower left indicates the power supply status the upper right indicates the module status Status indicator green yellow red Line power switch with green light 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 84 1260 Capillary Pump User Manual Troubleshooting and Diagnostics 6 Module Status Indicator The module status indicator indicates one of six possible module conditions e 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 e A green status indicator indicates the module is performing an analysis run mode A yellow indicator indicates a not ready condition The module is ina not ready state when it is waiting for a specific condition to be reached or completed for example immediately after changing a set point or while a self test procedure is running e An error condition is indicated when the status indicator is red An error condition indicates the module has detected an internal problem which affects correct operation of the module Usually an error condition requires attention e g leak defective internal components An error condition always interrupts the analysis A red blinking modules with on board LAN or
59. ce routines for all the maintenance routines The Agilent Lab Advisor software also allows users to monitor the status of their LC instruments The Early Maintenance Feedback EMF feature helps to carry out preventive maintenance In addition users can generate a status report for each individual LC instrument The tests and diagnostic features as provided by the Agilent Lab Advisor software may differ from the descriptions in this manual For details refer to the Agilent Lab Advisor software help files This manual provides lists with the names of Error Messages Not Ready messages and other common issues 1260 Capillary Pump User Manual 87 6 Troubleshooting and Diagnostics Agilent Lab Advisor Software 88 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual 7 Error Information What Are Error Messages 91 General Error Messages 92 Timeout 92 Shut Down 92 Remote Timeout 93 Synchronization Lost 93 Leak Sensor Short 94 Leak Sensor Open 94 Compensation Sensor Open 95 Compensation Sensor Short 95 Fan Failed 96 Leak 96 Module Error Messages 97 Zero Solvent Counter 97 Pressure Above Upper Limit 97 Pressure Below Lower Limit 98 Pressure Signal Missing 99 Valve Failed 99 Missing Pressure Reading 100 Pump Configuration 100 Valve Fuse 101 Inlet Valve Fuse 101 Temperature Out of Range 102 Temperature Limit Exceeded 102 Motor Drive Power 103 Encoder Missing 104 Inlet Valve Missing 104 Electro Magnetic Proportional V
60. ch power cord is different and designed to match the wall socket of a particular country or region Absence of ground connection or use of unspecified power cord The absence of ground connection or the use of unspecified power cord can lead to electric shock or short circuit gt Never operate your instrumentation from a power outlet that has no ground connection gt Never use a power cord other than the Agilent Technologies power cord designed for your region Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury gt Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Unintended use of supplied power cords Using power cords for unintended purposes can lead to personal injury or damage of electronic equipment gt Never use the power cords that Agilent Technologies supplies with this instrument for any other equipment 1260 Capillary Pump User Manual 35 2 Site Requirements and Specifications 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 8 1 inches in the rear for air circulation and electric connections If the bench should carry an Agilent s
61. ctor 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 Probable cause 1 Not ready condition in one of the instruments connected to the remote line 2 Defective remote cable 3 Defective components in the instrument showing the not ready condition Synchronization Lost Suggested actions Ensure the instrument showing the not ready condition is installed correctly and is set up correctly for analysis Exchange the remote cable Check the instrument for defects refer to the instrument s documentation During an analysis the internal synchronization or communication between one or more of the modules in the system has failed The system processors continually monitor the system configuration If one or more of the modules is no longer recognized as being connected to the system the error message is generated Probable cause 1 CAN cable disconnected 2 Defective CAN cable 3 Defective main board in another module 1260 Capillary Pump User Manual Suggested actions Ensure all the CAN cables are connected correctly Ensure all CAN cables are installed correctly Exchange the CAN cable Switch off the system Restart the system and determine which module or modules are not recognized by the system 93 7 94 Error Information Leak Sensor Short The l
62. d Due to the much smaller flow rates the Nanoflow pump does not have a mixer The mixer output flow called main flow is connected to the Electronic Flow Control EFC system The EFC system consists of an Electro Magnetic Proportioning Valve EMPV in series with a flow sensor The EMPV is protected from particles in the mobile phase by a solvent filter frit Responding to user entered column flow setpoint the EFC system determines how much of the main flow volume is ultimately delivered to the column The remaining main flow volume which is not required by the column is diverted to waste by the EMPV Under user control the EMPV can also function as a purge valve for purposes of solvent changeover etc In this case the EMPV is totally open and the total main flow is diverted to waste 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Capillary Pump 1 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 The gear train moves the two ball screw drives in opposite directions 180 degree out of phase The gear ratios are designed such that the first ball screw drive constantly moves at twice the speed of th
63. e written agreement with warranty terms covering the material in this document that conflict with these terms the warranty terms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcon tract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commercial item as defined in FAR 2 101 a or as Restricted computer soft ware as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or dis closure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly per formed or adhered to could result
64. e EMF Limits The setting of the EMF limits must be optimized over one or two maintenance cycles Initially no EMF limit should be set When performance indicates maintenance is necessary take note of the values displayed by Pump Liquimeter and Seal Wear Counters Enter these values or values slightly less than the displayed values as EMF limits and then reset the EMF counters to zero The next time the EMF counters exceed the new EMF limits the EMF flag will be displayed providing a reminder that maintenance needs to be scheduled 1260 Capillary Pump User Manual Maintenance 9 Checking and Cleaning the Solvent Inlet Filters When Parts required Preparations If solvent filter is blocked Description Concentrated nitric acid 65 Bidistilled water Beaker 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 The handling of toxic and hazardous solvents and reagents can bear health risks gt Please observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used CAUTION Small particles can permanently block the capillaries and valves of the module Damage of the module gt Always filter solvents
65. e Instant Pilot into any available CAN port of the 1260 system 5 Plug a CAN cable into the CAN connector of the Instant Pilot The Micro Online Degasser must not be connected to LAN or CAN as its connector is for diagnostic use only 6 Connect the CAN cable to the CAN connector of one of the modules 7 Press in the power switches to turn on the modules For more information about connecting the control module or Agilent control software refer to the respective user manual For connecting the Agilent 1260 Infinity equipment to non Agilent equipment see Introduction to the Pump on page 8 1260 Capillary Pump User Manual 53 3 Installing the Module Flow Connections Parts required p n Description 1 Other modules 1 G1376 68755 Accessory Kit 1 G2226 68755 Accessory Kit Nano Pump 2 wrenches 1 4 5 16 inch for capillary connections Preparations Pump is installed in the LC system WARNING When opening capillary or tube fittings solvents may leak out The handling of toxic and hazardous solvents and reagents can bear health risks gt Please observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used 54 1260 Capillary Pump User Manual Installing the Module 3 1 Remove the front cover by pressing the snap fasteners on both sides
66. e is optimized for the flow rate in use A change to larger stroke volumes is possible but not recommended When the pump is in the standard mode the EMPV is fully closed Total main flow up to 2500 uL min is directed to the LC system Column flow measurement control is disabled This mode is for non capillary LC applications In the capillary mode the standard flow sensor measures and controls column flow in the range of 1 20 uL min An extended range flow sensor optional provides flow measurement and control in the range of 10 100 L min Flow measurement is based on the principle of mass flow temperature sensitivity The flow sensor consists of a heated tube with two temperature sensors As the mobile phase passes through the heated tube the temperature characteristic distributed over the two temperature sensors is evaluated From the temperature characteristic flow rate accuracy is determined The flow sensor measurement is calibrated for specific mobile phases which are user selectable 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Capillary Pump 1 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 The early maintenance feedback EMF feature monitors the usage
67. e next module see Figure 8 on page 46 5 Press in the power switches to turn on the modules Connecting a Vacuum Degasser 1 Place the vacuum degaser in the stack of modules as shown in Figure 7 on page 45 2 Ensure the power switch at the front of the vacuum degasser is OFF switch stands out 3 Plug an APG cable into the APG remote connector at the rear of the degasser 4 Connect the APG cable to the APG remote connector of the pump see Figure 8 on page 46 5 Press in the power switch to turn on the vacuum degasser The AUX output is intended for troubleshooting It provides a DC voltage in the range of 0 1 V which is proportional to the vacuum level in the degasser chambers 52 1260 Capillary Pump User Manual Installing the Module 3 Connecting Control Software and or G4208 A Instant Pilot With the introduction of the Agilent 1260 Infinity all GPIB interfaces have been removed The preferred communication is LAN 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 1 Ensure the power switches on the front of the modules in the stack are OFF switches stand out 2 If there are no other 1260 with LAN port in the HPLC stack install a G1369B LAN board into the extension slot of the pump 3 Connect the LAN enabled module with a LAN cable to the data system 4 Plug the CAN connector of th
68. e second ball screw drive The servo motor includes a high resolution shaft position encoder which continuously reports the speed and direction of the motor in real time This speed and direction information is used by the pump control electronics to ensure precise control of the servo motor movement Each pump head consists of two identical chambers pistons and seals plus an active inlet valve and an outlet valve The solvent volume in each chamber is displaced by its piston The pistons are directly moved by the reciprocating ball screw drives of the metering drive assembly Due to the gear design of the metering drive assembly the pistons move in opposite directions with piston 1 constantly moving at twice the speed of piston 2 The outer diameter of the piston is smaller than the inner diameter of the chamber allowing solvent to flow in the gap between the piston and the chamber wall The two chambers are connected by the pressure dependent outlet valve The position of the solvent selection valve determines which of two solvents will be sucked low pressure through the active inlet valve into chamber 1 during the intake stroke of piston 1 The active inlet valve is electrically opened and closed making its operation more precise at low pressures The stroke volume of piston 1 is between 2 uL and 100 uL depending on flow rate When the pump is first turned on the user is prompted to initialize the pump The initialization routine occ
69. ead missing 107 pump housing parts 160 pump seals 132 148 purge valve 132 144 radio interference 191 reassembling the pump head 154 recommended pH range 38 remote cable 176 removing the pump head 146 repairs replacing firmware 15 7 157 results pressure test 119 RS 232C cable 183 communication settings 28 running the leak test 122 running the pressure test 118 S safety class 186 safety information lithium batteries 190 safety general information 186 standards 37 symbols 188 screwdriver pozidriv 1 148 screwdriver pozidriv 1 144 153 seal wear counter 149 seal wear counters 135 seal alternative material 75 seals 132 security lever 50 selection valve failed 99 selection valve fuse 101 serial number information 17 servo restart failed 106 setable flow range 38 shut down 92 sieve 132 142 site requirements power cords 35 snap fastener 55 solvent cabinet parts 163 solvent selection valve 144 solvent cabinet 62 solvent filters cleaning 138 solvent information 62 64 solvents 193 197 Index sonic bath 142 W sound emission 192 water Ai special interfaces 24 Wwashseals 132 special settings boot resident 30 forced cold start 31 wash seals 153 waste electrical and electronic specification equipment 189 rieg 38 WEEE directive 189 physica weight 37 wrench 1 4inch 118 122 142 148 wrench 14mm 139 140 140 142 wrench 1 4inch 146 stack configuration 48 rearview 48 status ind
70. eak 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 1 Defective flow sensor 2 Leak sensor incorrectly routed being pinched by a metal component Leak Sensor Open Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative The leak sensor in the module has failed open 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 falls outside the lower limit the error message is generated Probable cause 1 Leak sensor not connected to the main board 2 Defective leak sensor 3 Leak sensor incorrectly routed being pinched by a metal component Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative 1260 Capillary Pump User Manual Error Information 7 Compensation Sensor Open The ambient compensation sensor NTC on the main board in the module has failed open circuit The resistance acr
71. epresentative 2 Defective fan Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative 4 Improperly positioned cables or wires Ensure the fan is not mechanically blocked obstructing fan blades A leak was detected in the module The signals from the two temperature sensors leak sensor and board mounted temperature compensation sensor are used by the leak algorithm to determine whether a leak is present When a leak occurs the leak sensor is cooled by the solvent This changes the resistance of the leak sensor which is sensed by the leak sensor circuit on the main board Probable cause Suggested actions 1 Loose fittings Ensure all fittings are tight 2 Broken capillary Exchange defective capillaries 3 Loose or leaking active inlet valve outlet ball Ensure pump components are seated correctly valve or EMPV If there are still signs of a leak exchange the appropriate seal active inlet valve outlet ball valve or EMPV 4 Defective pump seals Exchange the pump seals 1260 Capillary Pump User Manual Module Error Messages Zero Solvent Counter Error Information 7 The error message is triggered if the remaining volume in a solvent bottle falls below the set limit Probable cause 1 Volume in bottle below specified volume 2 Incorrect setting Pressure Above Upper Limit Suggested actions Refill bottles and reset solvent counters
72. er T ENX c S 7 E oo T 2 I Sais Thermostat for the ALS optional Solvent cabinet Degasser optional Pump Figure 9 Recommended Two Stack Configuration for 1260 Front View 1260 Capillary Pump User Manual 47 3 Installing the Module Optimizing the Stack Configuration LAN to control software CAN Bus cable to Instant Pilot Thermo cable optional ae Remote cable AC Power CAN Bus cable AC Power Figure 10 Recommended Two Stack Configuration for 1260 Rear View 48 1260 Capillary Pump User Manual Installing the Module 3 Installing the Pump Parts required Preparations p n Description 1 Pump 1 Data System 1 G4208A Instant Pilot 1 Power cord For other cables see text below and Cable Overview on page 172 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 shock hazard when the cover is opened and the module is connected to power gt Make sure that it is always possible to acce
73. er Manual Suggested actions Ensure the solvent selection valve is connected correctly Ensure the connection cable is connected correctly Exchange the connection cable Exchange the solvent selection valve 99 7 Error Information 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 Ims 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 3 Defective main board Please contact your Agilent service representative Pump Configuration At switch on the pump has recognized a new pump configuration The pump is assigned its configuration at the factory If the active inlet valve and pump encoder of channel B are disconnected and the pump is rebooted the error message is generated However the pump will function as an isocratic pump in this configuration The error message reappears after each switch on Probable cause Suggested actions 1 Active inlet valve and pump encoder of Reconnect the active inlet valve and pump channel B disconnected encoder of channel B 100 1260 Capillary Pump User Manual Error Information 7 Valve Fuse Valve Fuse 0 Channels Al and A2 Valve Fuse 1 Ch
74. erated Possible Reasons for a Wait Timeout Pressure not reached Pump channel A did not reach the delivery phase Pump channel B did not reach the delivery phase Pump channel A did not reach the take in phase Pump channel B did not reach the take in phase Solvent volume not delivered within the specified time Probable cause Suggested actions 1 System still in purge mode Ensure that purge valve is closed 2 Leak at fittings EMPV active inlet valve Ensure pump components are seated correctly outlet valve or piston seals If there are still signs of a leak exchange the appropriate seal purge valve active inlet valve outlet valve piston seal 3 Flow changed after starting test Ensure correct operating condition for the special application in use 4 Defective pump drive assembly Please contact your Agilent service representative 110 1260 Capillary Pump User Manual Error Information 7 Electronic fuse of SSV The electronic fuse protecting the solvent selection valve electronics has blown Probable cause Suggested actions 1 Recoverable error of the SSV electronic Restart module the electronic fuse can recover If not contact Agilent service 2 Short cut of SSV cable Replace cable between board and SSV 1260 Capillary Pump User Manual 111 7 Error Information Module Error Messages 112 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual 8 Test Functions and Calibration
75. esponse The detector is used at medium or low sensitivity Removing the mixer will result in an increase of the composition wander and higher detector noise The Standard Filter The standard filter has a volume of typically 100 uL If the application needs a reduced volume e g for fast gradient the use of the Universal solvent filter kit 20 uL p n 01090 68703 is recommended Be aware that the filter efficiency and capacity is significantly reduced compared to the standard one Never run the pump without an inline filter 1260 Capillary Pump User Manual 77 5 Optimizing Performance How to Optimize the Compressibility Compensation Setting 78 The compressibility compensation default settings are 50 x 10 bar best for most aqueous solutions for pump head A and 115 x 106 bar to suit organic solvents for pump head B The settings represent average values for aqueous solvents A side and organic solvents B side Therefore it is always recommended to use the aqueous solvent on the A side of the pump and the organic solvent on the B side Under normal conditions the default settings reduce the pressure pulsation to values below 1 of system pressure which is sufficient for most applications If the compressibility values for the solvents used differ from the default settings it is recommended to change the compressibility values accordingly Compressibility settings can be optimized by using the values for various sol
76. he EMPV is suspected of being leaky or contaminated with particles The outlet of the EMPV is plugged with an SST blank nut After a short flushing routine the EMPV is closed and the pressure is increased to approximately 380 bar The EMPV is then opened and the pressure is released very quickly This procedure is repeated several times in a sequence Running the Test 1 oo uy OO 1 A 128 Fill vacuum degasser channel Al and B1 with solvents the test requires filled vacuum chambers We recommend that you use channel A with aqueous solvent If you use a different channel you must ensure the miscibility of the solvent that no precipitation of buffer occurs Plug the pump outlet with blank nut at EMPV outlet Disconnect the EMPV to flow sensor at the EMPV outlet Plug the EMPV outlet port with blank nut 01080 83202 Execute test Check result with Pressure Test if necessary Remove the blank nut Reconnect the EMPV to flow sensor capillary Do not overtighten 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual ee 9 e Maintenance J Introduction to Maintenance 130 Warnings and Cautions 131 Overview of Maintenance 132 Cleaning the Module 134 Early Maintenance Feedback EMF 135 EMF Counters 135 Using the EMF Counters 136 Checking and Cleaning the Solvent Inlet Filters 137 Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve 139 Removing the Active Inlet Valve 139
77. he Purge Mode and set the flow rate to 2 5 ml min 2 Flush the vacuum degasser and all tubes with at least 5 ml of solvent 3 Set flow to required value of your application and activate the pump micro mode 4 Pump for approximately 5 minutes before starting your application 5 Repeat step 1 on page 59 through step 2 on page 59 for the other channel s of the pump When the pumping system has been turned off for a certain time for example overnight oxygen will re diffuse into the solvent channel between the vacuum degasser and the pump Solvents containing volatile ingredients will slightly lose these if left in the degasser without flow for a prolonged period of time Therefore purging each channel at 2 5 ml min for 1 minute is required before starting an application 1260 Capillary Pump User Manual 59 3 Installing the Module Get the System Ready for the First Injection 60 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual 4 Using the Pump Hints For Successfully Using the Pump 62 Solvent Information 64 Algae Growth in HPLC Systems 65 How to Prevent and or Reduce the Algae Problem 66 Inject the Check out Sample 67 Conditions 67 Procedure 68 Typical Chromatogram 68 Checkout procedure for a G2229A Nano LC System 69 Method Parameters 70 Test Results and Evaluation 72 This chapter provides advice for the successful operation of the 1260 Series Capillary Pump and the checkout procedure for Agilent capillary HPLC
78. he aqueous solvent in channel A and the organic solvent in channel B The default compressibility and flow sensor calibration settings are set accordingly Always use the correct calibration values For generation of fast gradients on short columns remove the mixer enter the new pump configuration and select the fast gradient range for the primary flow rate chromatographic performance will not be impacted When running in Micro Mode check the correct instrument setup flow sensor type used mixer and filter 1260 Capillary Pump User Manual Usingthe Pump 4 Fused Silica Capillary Issues e 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 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 e Be careful when bending fused silica capillaries The diameter must not be smaller than 40 mm 40 mm When you replace a part especially a capillary clean it with acetone If a fused silica capillary leaks do not retighten the fitting under flow Set the column flow to zero re insert the capillary tighten and set the new column flow e Avoid the use of alkaline solutions pH gt 8 5 as they attack the fused silica of the capillarie
79. he volume displaced into the system will be reduced by the compressed volume When a compressibility compensation value for a pump head is set the pump processor calculates a compensation volume that depends on the system pressure and the selected compressibility value This compensation volume is added to the delivery stroke of the first piston 1260 Capillary Pump User Manual 13 1 14 Introduction to the 1260 Infinity Capillary 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 Small stroke volumes will generate less pressure pulsations than higher stroke volumes at same flow rates In addition the frequency of the pressure pulsations will be higher This will decrease the influence of flow pulsations on quantitative results In gradient mode smaller stroke volumes resulting in less flow ripple will improve composition ripple The pump uses a processor controlled ball screw system to drive its pistons The normal stroke volume is optimized for the selected flow rate Small flow rates use a small stroke volume while higher flow rates use a higher stroke volume The stroke volume for the pump is set to AUTO mode This means that the strok
80. icator 85 stroke length 109 stroke volume 14 Z synchronization lost 93 system setup and installation optimizing stack configuration 44 zero solvent counter 97 T temperature limit exceeded 102 temperature out of range 102 temperature sensor 96 test functions 82 timeout 92 tools screwdriver pozidriv 1 148 screwdriver pozidriv 1 144 153 wrench 1 4 inch 148 troubleshooting error messages 82 91 status indicators 82 84 V vacuum degasser 52 variable stroke volume 14 voltage range 37 198 1260 Capillary Pump User Manual www agilent com In This Book This manual contains technical reference information about the Agilent 1260 Infinity Capillary Pump G1376A The manual describes the following introduction to the pump requirements and specifications e installation using the pump e optimizing performance e troubleshooting and diagnostics maintenance e parts and materials e overview of cables legal safety and warranty information Agilent Technologies 2007 2008 2010 Printed in Germany 06 2010 G1376 90014 fe Agilent Technologies
81. icro pressure test with port 6 of the autosampler valve blanked off 6 Install the restriction capillary to port 6 of the autosampler injection valve 7 Pump 1 5 uL min micro mode 70 A water 30 B acetonitrile Pump as long as it takes for the pressure to get stable Continue pumping for at least 5 min more before continuing 1260 Capillary Pump User Manual 69 4 70 Using the Pump Method 8 Pump 0 6 uL 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 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 Parameters Method Parameters Nanoflow Pump Table 17 Method Parameters for Nanoflow Pump Parameter Value Column flow 0 6 pL min Stoptime 15 min Solvent A 70 Solvent B 30 Calibrated as H 0 ACN Primary flow 200 500 pL min Compressibility A 50 10 bar Compressibility B 115 10 bar Min stroke A and B Auto Fast composition change ON 1260 Capillary Pump User Manual Using the Pump 4 Table 18 Timetable Time 0 00 3 00 3 01 6 00 6 01 9 00 9 01 12 00 12 01 15 00 min Flow 0 6 0 6 0 3 0 3 0 6 0 6 0 3 0 3 0 6 0 6 uL mi n Method Parameters Micro High Performance Autosampler Injection volume 0 000
82. illary Pump 1 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 gt Save your methods and data before executing a forced cold start If you use the following switch settings and power the instrument up again a forced cold start has been completed Table 12 Forced Cold Start Settings without on board LAN Mode Select SW1 sw2 SW3 sw4 SW5 SW6 SW7 Sws LAN TEST BOOT 1 1 0 0 0 0 0 1 No LAN TEST BOOT 1 1 0 0 1 0 0 1 1260 Capillary Pump User Manual 31 1 32 Introduction to the 1260 Infinity Capillary Pump Setting the 8 bit Configuration Switch On Board LAN 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual 6 ee 2 e Site Requirements and Specifications 8 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 Capillary Pump ee Agilent Technologies 33 2 Site Requirements and Specifications Site Requirements A suitable environment is important to ensure optimal performance of the instrument Power Considerations The module power supply has wide ranging capability I
83. in damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated condi tions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indi cated conditions are fully under stood and met 1260 Capillary Pump User Manual Contents Contents 1 Introduction to the 1260 Infinity Capillary Pump 7 Introduction tothe Pump 8 Early Maintenance Feetback 15 Instrument Layout 16 Electrical Connections 17 Interfaces 19 Setting the 8 bit Configuration Switch On Board LAN 25 2 Site Requirements and Specifications 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 Control Software 52 Flow Connections 54 Get the System Ready for the First Injection 58 4 Usingthe Pump 61 Hints For Successfully Using the Pump 62 Solvent Information 64 Algae Growth in HPLC Systems 65 Inject the Check out Sample 67 Checkout procedure fora G2229A NanoLC System 69 5 Optimizing Performance 73 Hints for the Micro Vacuum Degasser 74 Choosing the Right Pump Seals 75 How to Choose the Primary Flow 76 1260 C
84. ings for the modules without on board LAN only 1260 Capillary Pump User Manual 27 1 28 Introduction to the 1260 Infinity Capillary Pump Table 6 8 bit Configuration Switch without on board LAN Mode Select 1 2 3 4 5 6 7 8 RS 232C 0 1 Baudrate Data Parity Bits Reserved 1 0 Reserved TEST BOOT 1 1 rsvo sys rsvo_ Rsvo FC The LAN settings are done on the LAN Interface Card G1369A B Refer to the documentation provided with the card Communication Settings for RS 232C The communication protocol used in the column compartment supports only hardware handshake CTS RTR Switches 1 in down and 2 in up position define that the RS 232C parameters will be changed Once the change has been completed the column instrument must be powered up again in order to store the values in the non volatile memory Table 7 Communication Settings for RS 232C Communication without on board LAN Mode Select 1 2 3 4 5 6 7 8 RS 232C 0 1 Baudrate Data Bits Parity Use the following tables for selecting the setting which you want to use for RS 232C communication The number 0 means that the switch is down and 1 means that the switch is up 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Capillary Pump 1 Table 8 Baudrate Settings without on board LAN Switches Baud Rate Switches Baud Rate 3 4 5 3 4 5 0 0 0 9600 1 0 0 9600 0 0 1 1200 1 0 1 14400 0 1 0 2400 1 1 0 19200 0 1 1 4
85. ition 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 Probable cause Suggested actions 1 Defective pump drive assembly Please contact your Agilent service representative Initialization Failed Initialization Failed Pump channel A B Initialization Failed Pump channel B The module failed to initialize successfully within the maximum time window A maximum time is assigned for the complete pump initialization cycle If the time is exceeded before initialization is complete the error message is generated Probable cause Suggested actions 1 Blocked passive inlet valve Exchange the inlet valve 2 Defective pump drive assembly Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative 1260 Capillary Pump User Manual 109 7 Error Information 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 gen
86. lary Pump Accessory Kit 169 1 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 184 12 Appendix 185 General Safety Information 186 The Waste Electrical and Electronic Equipment Directive 189 Batteries Information 190 Radio Interference 191 Sound Emission 192 Solvent Information 193 Agilent Technologies on Internet 194 1260 Capillary Pump User Manual Contents 6 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual 1 Introduction to the 1260 Infinity Capillary Pump Introduction tothe Pump 8 Hydraulic Path Overview 10 How Does the Pumping Unit Work 11 How Does Compressibility Compensation Work 13 How Does Variable Stroke Volume Work 14 Early Maintenance Feetback 15 Instrument Layout 16 Electrical Connections 17 Serial Number Information ALL 17 Rear View of the Module 18 Interfaces 19 Overview Interfaces 21 Setting the 8 bit Configuration Switch On Board LAN 25 Communication Settings for RS 232C 28 Special Settings 30 This chapter provides an introduction to the operation principles of the capillary pump and the electrical interfaces att Agilent Technologies 7 1 Introduction to the 1260 Infinity Capillary Pump Introduction to the Pump The low flow pumps consist of two identical pumping units in a single housing They gener
87. livers with a flow rate of 3 uL min for 30 s Ramp 5 Piston A1 delivers 50 uL min for approximately 8 s Plateau 3 Piston A1 delivers with a flow rate of 3 uL min for 30 s Ramp 6 Piston B1 delivers 50 uL min for approximately 7 s Plateau 4 Piston B1 delivers with a flow rate of 3 uL min for approximately 30 s At the end of the fourth plateau the test is finished and the pump switches off 1260 Capillary Pump User Manual 121 8 Test Functions and Calibration Running the Leak Test When Tools required Parts required Preparations 122 If problems with the pump are suspected Wrench 1 4 inch p n Description 1 G1313 87305 Restriction Capillary 1 01080 83202 Blank nut 1 500 ml lsopropanol 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 Move the inline filter outlet capillary from the EMPV to to manual purge valve Make absolutely sure that all parts of the flow path that are part of the test are very thoroughly flushed with IPA before starting to pressurize the system Any trace of other solvents or the smallest air bubble inside the flow path definitely will cause the test to fail Running the test from the Agilent Lab Advisor software 1 Select the Leak Test from the Test Selection menu 2 Start the test and follow the instructions
88. ng conditions the radio interference limits are still met within the premises 1260 Capillary Pump User Manual 191 12 Appendix Sound Emission Manufacturer s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991 This product has a sound pressure emission at the operator position lt 70 dB e Sound Pressure Lp lt 70 dB A e At Operator Position e Normal Operation e According to ISO 7779 1988 EN 27779 1991 Type Test 192 1260 Capillary Pump User Manual Appendix 12 Solvent Information Observe the following recommendations on the use of solvents e Brown glass ware can avoid growth of algae e Small particles can permanently block capillaries and valves Therefore always filter solvents through 0 4 um filters e Avoid the use of the following steel corrosive solvents Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like sulfuric acid and nitric acid especially at higher temperatures if your chromatography method allows replace by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2CHCly O gt gt 2COCl 2HC1 This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chlor
89. nnect the valve capillary from the outlet valve 2 Using the 14 mm wrench loosen the valve and remove it from the pump body 3 Remove the plastic cap with the gold seal from the outlet valve 4 Using a pair of tweezers remove the sieve Check the gold seal It should be exchanged when strongly deformed Place the valve in an upright position insert the sieve into the recess and replace the gold seal with the cap Make sure that the sieve cannot move and is away from the seal area of the gold seal 5 Place a new sieve into the recess of the outlet valve and replace the cap with the gold seal 1260 Capillary Pump User Manual Maintenance Exchanging the Outlet Valve Sieve 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 Valve body Gold seal Plastic cap S Figure 20 Outlet Ball Valve Parts 7 Reinstall the outlet valve and tighten the valve 8 Reconnect the valve capillary Valve capillary Outlet ball valve Figure 21 Exchanging the Outlet Valve 1260 Capillary Pump User Manual 143 9 Maintenance 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 gt Position the solvent bottles at a level below the pump to av
90. of specific components in the instrument and provides feedback when the user selectable limits have been exceeded The visual feedback in the user interface provides an indication that maintenance procedures should be scheduled EMF Counters EMF counters increment with use and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded Some counters can be reset to zero after the required maintenance procedure 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 useful maintenance cycle is dependent on the requirements for use Therefore the definition of the maximum limits need to be determined based on the specific operating conditions of the instrument Setting the EMF Limits The setting of the EMF limits must be optimized over one or two maintenance cycles Initially the default EMF limits should be set When instrument performance indicates maintenance is necessary take note of the values displayed by the EMF counters Enter these values or values slightly less than the displayed values as EMF limits and then reset the EMF counters to zero The next time the EMF counters exceed the new EMF limits the EMF flag will be displayed providing a reminder that maintenance needs to be scheduled 1260 Capillary Pump User Manual 15 1 Introduction to the 1260 Infinity Capillary
91. oform if the drying process removes the stabilizing alcohol Chromatographic grade ethers which can contain peroxides for example THF dioxane di isopropylether such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides Solvents containing strong complexing agents e g EDTA Mixtures of carbon tetrachloride with 2 propanol or THF 1260 Capillary Pump User Manual 193 12 Appendix 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 194 1260 Capillary Pump User Manual Index Index 8 bottle head assembly parts 163 8 bit configuration switch buffer application 62 on board LAN 25 without On Board LAN 27 C cable A analog 174 accessory kit parts 43 169 BCD 179 CAN 181 active inlet valve 132 139 139 Agilent Diagnostic software 87 Agilent Lab Advisor software 87 connecting APG remote 48 connecting CAN 48 connecting GPIB 48 Agilent Lab Advisor 87 connecting LAN 48 Agilent connecting the ChemStation 48 oninternet 194 connecting the power 48 algae 193 external contact 182 alternative seal material 75 interface 51 ambient operating temperature 37 LAN 181 ambient non operating temperature 37 remote 176 analog output 39 RS 232 183 analog signal 22 cables analog analog 1 2
92. oid solvent spillage due to hydrostatic pressure 144 1260 Capillary Pump User Manual Maintenance 9 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 de H Solvent tubes eal au X ae masa ESN y E EER Solvent selection valve Connecting tubes Figure 22 Exchanging the solvent selection valve Using a Pozidriv screwdriver 1 loosen the holding screws of the valves Pull the valve module out and detach the connector Push the connector of the new solvent selection valve into the receptacle oa FF Ww N Fix the new valve with the two holding screws and reconnect the solvent lines 6 Connect the valve module to its electrical connectors and fix the assembly with the two holding screws 7 Reinstall solvent tubes and the active inlet valve connection tubes 1260 Capillary Pump User Manual 145 9 Maintenance 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 Switch off pump at power switch Remove the front cover to have access to the pump mechanics
93. or to be connected to Agilent modules The other end depends on the instrument to which connection is being made Agilent Module to 3394 6 Integrators p n 35900 60750 Pin 3394 6 Pin Agilent Signal Name module 1 Not connected 2 Shield Analog 3 Center Analog E57 1260 Capillary Pump User Manual Agilent Module to BNC Connector Identifying Cables 11 p n 8120 1840 Pin BNC Pin Agilent Signal Name module nn dl Shield Shield Analog lt _ EO Center Center Analog Agilent Module to General Purpose p n 01046 60105 Pin 3394 6 Pin Agilent Signal Name module 1 Not connected 2 Black Analog 3 Red Analog E xg 1260 Capillary Pump User Manual 175 11 Identifying Cables Remote Cables 176 O O JNE 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 Agilent Module to 3396A Integrators p n 03394 60600 Pin 3394 Pin Agilent Signal Name Active module TTL Z 9 1 White Digital ground a NC 2 Brown Prepare run Low 3 3 Gray Start Low z NC 4 Blue Shut down Low 5 NC 5 Pink Not connected i NC 6 Yellow Power on High o 5 14 7 Red Ready High 1 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent
94. ore information 1260 Capillary Pump User Manual 189 12 Appendix Batteries Information 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 gt Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries gt Replace only with the same or equivalent type recommended by the equipment manufacturer Lithiumbatteri Eksplosionsfare ved fejlagtig handtering Udskiftning ma kun ske med batteri af samme fabrikat og type gt Lever det brugte batteri tilbage til leverand ren Lithiumbatteri Eksplosionsfare Ved udskiftning benyttes kun batteri som anbefalt av apparatfabrikanten gt Brukt batteri returneres appararleverandoren 190 Bij dit apparaat zijn batterijen geleverd Wanneer deze leeg zijn moet u ze niet weggooien maar inleveren als KCA 1260 Capillary Pump User Manual Appendix 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 operati
95. osampler Special Interfaces Some modules have module specific interfaces connectors They are described in the module documentation 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Capillary Pump 1 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 G1315 65C D G1314D E F G4212A B G4220A e Default is ALL switches DOWN best settings Bootp mode for LAN e For specific LAN modes switches 3 8 must be set as required For boot test modes switches 1 2 must be UP plus required mode REMOTE Figure 5 Location of Configuration Switch example shows a G4212A DAD To perform any LAN configuration SW1 and SW2 must be set to OFF For details on the LAN settings configuration refer to chapter LAN Configuration 1260 Capillary Pump User Manual 25 1 Introduction to the 1260 Infinity Capillary Pump Table 5 8 bit Configuration Switch with on board LAN Mode Function SW 1 SW 2 SW 3 SW 4 SW 5 SW 6 SW7 SW 8 LAN 0 0 Link Configuration Init Mode Selection Auto negotiation 0 xX x x x x 10 MBit half duplex 1 0 0 X X xX 10 MBit full duplex 1 0 1 xX x xX 100 MBit half duplex 1 1 0 x X X 100 MBit
96. oss 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 Probable cause Suggested actions 1 Defective main board Please contact your Agilent service representative Compensation Sensor Short The ambient compensation sensor NTC on the main board in the module has failed short 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 falls below the lower limit the error message is generated Probable cause Suggested actions 1 Defective main board Please contact your Agilent service representative 1260 Capillary Pump User Manual 95 7 96 Error Information Fan Failed Leak 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 This limit is given by 2 revolutions second for longer than 5 seconds Probable cause Suggested actions 1 Fan cable disconnected Please contact your Agilent service r
97. pillary Pump User Manual Maintenance 9 Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve 4 Using the 14 mm wrench tighten the nut by turning the valve in its final position not more than a quarter turn Do not overtighten the valve The solvent inlet tube connection should point to the right corner of the pump head 5 Reconnect the inlet tube and the active inlet valve cable to the connector at the Z panel NOTE Make sure you are in normal mode 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 Active inlet valve Solvent inlet tube Figure 19 Exchanging the Active Inlet Valve 1260 Capillary Pump User Manual 141 9 Maintenance Exchanging the Outlet Valve Sieve When Tools required Parts required 142 Sieve whenever the pump seals will be exchanged Valve if internally leaking Wrench 1 4 inch Wrench 14 mm 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 Place the valve in upright position onto the plastic cap in a small beaker with alcohol Place in a sonic bath for 5 10 min Insert a new sieve and replace the gold seal 1 Using a 1 4 inch wrench disco
98. r Seal general purpose black pack of 2 Seal general purpose black pack of 2 Capillary outlet valve to piston 2 Pump head body 1260 Active inlet valve without cartridge Active Inlet Valve Cartridge 400 bar Outlet valve complete Screw lock Adapter Screw M5 60 mm long The complete pump head assembly includes items 1 4 6 9 and 11 166 1260 Capillary Pump User Manual Parts and Materials for Maintenance 10 Pump Head Assembly Figure 28 Pump Head Assembly 1260 Capillary Pump User Manual 167 10 Parts and Materials for Maintenance Flow Sensor Assembly Item p n Description 1 G1376 60001 Flow sensor 20 pL 1260 Capillary Pump G1376 60002 Flow sensor 100 pL 1260 Capillary Pump G1375 87301 Capillary EMPV to flow sensor 20 uL flow sensor G1375 87305 Capillary EMPV to flow sensor 100 uL flow sensor G1375 87310 Fused silica PEEK capillary 50 pm55 cm 20 pL flow sensor G1375 87306 Fused silica PEEK capillary 100 m55 cm 100 pL flow sensor Figure 29 Flow Sensor Assembly 168 1260 Capillary Pump User Manual Parts and Materials for Maintenance 10 Capillary Pump Accessory Kit Accessory Kit p n G1376 68755 p n 0515 0175 0890 1760 2x 2190 0586 5022 2185 5181 1519 01018 23702 01018 60025 4x 61311 60009 61312 23200 61315 45003 G1375 87310 8710 1534 8710 0806 2x G1376 90014 1260 Capillary Pump User Manual Description Mounting screw for manual purge valve holde
99. r M4 20 mm long Tubing Flexible 1 ea 1 meter Washer for purge valve holder screw Replacement SS frit 0 5 um pore size CAN cable Agilent module to module 1 m Insert tool Solvent inlet filter stainless steel Manual purge valve Holder for manual purge valve Torque adapter Fused silica PEEK capillary 50 pm55 cm 20 pL flow sensor Wrench 4 mm both ends open end Wrench open end 1 2 inch and 7 16 inch Agilent 1260 Infinity Capillary Pump User Manual 169 10 Parts and Materials for Maintenance Capillary Pump Accessory Kit 170 1260 Capillary Pump User Manual 1260 Capillary 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 182 Agilent Module to PC 183 Agilent 1200 Module to Printer 184 This chapter provides information on cables used with the Agilent 1200 Infinity Series modules ot Agilent Technologies 171 11 Identifying Cables Cable Overview 172 Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Analog cables p n Description 35900 60750 Agilent module to 3394 6 integrators 35900 60750 Agilent 35900A A D converter 01046 60105 Analog cable BNC to general purpose spade lugs Remote cables p n Description 03394 60600 Agilent module to 3396A Series integrators 3396 Series Il
100. rates up to 100 pL min and electronic flow control active primary flow path 180 480 pL without mixer 600 900 pL with mixer system pressure dependant Typically 180 480 uL system pressure dependent without mixer for flow rates up to 2 5 mL min Mixer delay volume 420 pL 20 400 bar 5880 psi system pressure User selectable based on mobile phase compressibility 1 0 8 5 solvents with pH lt 2 3 should not contain acids which attack stainless steel Upper pH range is limited by fused silica capillaries 38 1260 Capillary Pump User Manual Site Requirements and Specifications 2 Table 14 Performance Specification Agilent 1260 Infinity Capillary Pump G1376A Type Specification Control and data Agilent Control Software Chemstation EZ Chrom OL etc evaluation 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 Extensive diagnostics error detection and display though Instant Pilot and Data System leak maintenance detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas GLP features Early maintenance feedback EMF for continuous tracking of instrument usage in terms of seal wear and volume of pumped mobile phase with user settable limits and feedback messages Electronic records of main
101. re of leaking solvents 3 Using a 14 mm wrench loosen the active inlet valve and remove the valve from pump head Active inlet valve body Valve cartridge Figure 18 Active Inlet Valve Parts 1260 Capillary Pump User Manual 139 9 Maintenance Exchanging the Valve Cartridge When Tools required Parts required If internally leaking backflow Wrench 14 mm 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 3 Insert a new cartridge into the actuator assembly make sure the valve cartridge is completely inserted into the actuator assembly Replacing the Active Inlet Valve Body When Tools required Parts required 140 If leaking from the bottom of the active inlet valve body Ifthe soleniod is defective Wrench 14 mm 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 2 Insert the new valve into the pump head Using the 14 mm wrench turn the nut until it is hand tight 3 Position the valve so that the solvent inlet tube connection points towards the front 1260 Ca
102. reshold Shut Down Suggested actions Check the logbook for the occurrence and source of a not ready condition Restart the analysis where required Check the logbook for the occurrence and source of a not ready condition Restart the analysis where required An external instrument has generated a shut down signal on the remote line The module continually monitors the remote input connectors for status signals A LOW signal input on pin 4 of the remote connector generates the error message Probable cause 1 Leak detected in another module with a CAN connection to the system 2 Leak detected in an external instrument with a remote connection to the system 3 Shut down in an external instrument with a remote connection to the system 4 The degasser failed to generate sufficient vacuum for solvent degassing Suggested actions Fix the leak in the external instrument before restarting the module Fix the leak in the external instrument before restarting the module Check external instruments for a shut down condition Check the vacuum degasser for an error condition Refer to the Service Manual for the degasser or the 1260 pump that has the degasser built in 1260 Capillary Pump User Manual Remote Timeout Error Information 7 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 dete
103. restriction capillary Tighten the active inlet valve in channel A 14 mm wrench Do not overtighten Ensure the pump head screws in channel A are tight Ensure the sieve in the outlet valve is installed correctly Tighten the outlet valve Exchange the pump seals in channel A Check the pistons for scratches Exchange if scratched Exchange the active inlet valve in channel A Fourth plateau negative or unstable and at least one other plateau positive Probable cause 1 Airin pump chamber of channel B or seals not yet seated 2 Loose active inlet valve in channel B 3 Loose pump head screws in channel B 4 Loose outlet valve in channel B 5 Leaking seal or scratched piston in channel B1 6 Defective active inlet valve in channel B Suggested actions Flush channel B thoroughly with isopropanol under pressure restriction capillary Tighten the active inlet valve in channel B 14mm wrench Do not overtighten Ensure the pump head screws in channel B are tight Ensure the sieve in the outlet valve is installed correctly Tighten the outlet valve Exchange the pump seals in channel B Check the pistons for scratches Exchange if scratched Exchange the active inlet valve in channel B 1260 Capillary Pump User Manual Test Functions and Calibration 8 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
104. rge leaks visible at the pump seals Exchange the pump seals 5 Large leaks visible at active inlet valve or Ensure the leaky components are installed outlet valve tightly Exchange the component if required 1260 Capillary Pump User Manual 123 Test Functions and Calibration Pressure limit not reached but plateaus horizontal or positive Probable cause 1 Degasser and pump channels A and or B not flushed sufficiently air in the channels 2 Wrong solvent All plateaus negative Probable cause 1 Loose or leaky fittings 2 Leaky mixer if installed 3 Loose pump head screws in channel A or B 4 Leaking seal or scratched piston in channel A2 or B2 5 Leaking outlet valve in channel A or B 6 Leaky damper Suggested actions Purge the degasser and pump channels thoroughly with isopropanol under pressure use the restriction capillary Install isopropanol Purge the degasser and pump channels thoroughly Suggested actions Ensure all fittings are tight or exchange capillary Tighten the mixer fittings and nuts Ensure the pump head screws in channels A and B are tight Exchange the pump seals in both channels Check the pistons for scratches Exchange if scratched Exchange the outlet valve Exchange damper 1260 Capillary Pump User Manual Test Functions and Calibration First plateau negative or unstable and at least one other plateau positive Probable cause 1 Leaking outlet
105. rts 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 5 6 mm long for Housing Front 2x Figure 25 Overview of Main Assemblies Rear View 162 1260 Capillary Pump User Manual Parts and Materials for Maintenance 10 Solvent Cabinet and Bottle Head Assembly Item p n 1 5065 9981 2 5042 8901 5043 0207 3 5065 9954 4 5042 8567 G1311 60003 5 6 01018 60025 7 5062 2483 5063 6598 5063 6599 9301 1420 9301 1450 Description Solvent cabinet including all plastic parts Name plate Name plate 1260 Front panel solvent cabinet Leak pan Bottle head assembly Solvent inlet filter stainless steel Solvent tubing 5 m Ferrules with lock ring 10x Tube screw 10x Solvent bottle transparent Solvent bottle amber r 2 j C 5 6 Figure 26 1260 Capillary Pump User Manual Solvent Cabinet Parts 163 10 Parts and Materials for Maintenance Hydraulic Path Item p n 1 G1311 60003 2 G1311 67304 3 G1312 67300 4 G1312 67304 5 G1312 67302 6 01090 87308 7 G1312 87330 01090 87308 9 5064 8273 5022 2185 10 61375 87400 11 61375 87301 61375 87305 12 G1375 87310 G1375 87306 5062 2463
106. s Be careful not to crush capillaries when closing module doors A broken capillary can release silica particles into the system e g cell causing problems in the system downstream of the crack Often a clogged capillary can be recovered by backflushing with acetone 1260 Capillary Pump User Manual 63 4 Using the Pump Solvent Information Always filter solvents through 0 4 um filters small particles can permanently block the capillaries and valves Avoid the use of the following steel corrosive solvents 64 Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like sulfuric and nitric acid especially at higher temperatures replace if your chromatography method allows by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2CHCly Os gt 2COCly 2HC1 This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol Chromatographic grade ethers which can contain peroxides for example THF dioxane di isopropylether Such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides Solvents containing strong complexing agents e g EDTA Mixtures of carbon tetrachloride
107. sassemble the pump head assembly of the leaky pump head see Removing and Disassembling the Pump Head on page 146 2 Using one of the pistons carefully remove the seal from the pump head be careful not to break the piston Remove wear retainers if still present Piston g LAA E 7 Seal A 148 1260 Capillary Pump User Manual 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 139 and Exchanging the Outlet Valve Sieve on page 142 and the capillary Inject solvent into each chamber Chambers 4 Insert seals into the pump head and press firmly in position Seal 5 Reassemble the pump head assembly see Reassembling the Pump Head Assembly on page 154 Reset theseal wear counter and liquimeter as described in the User Interface documentation 1260 Capillary Pump User Manual 149 9 Maintenance Seal Wear in Procedure 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
108. 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 Liquimeters The liquimeters display the total volume of solvent pumped by the left and right pump heads since the last reset of the counters Both liquimeters can be assigned an EMF maximum limit When the limit is exceeded the EMF flag in the user interface is displayed Seal Wear Counters The Seal Wear Counters display a value derived from pressure and flow both contribute to seal wear The values increment with pump usage until the 1260 Capillary Pump User Manual 135 9 136 Maintenance counters are reset after seal maintenance Both Seal Wear Counters can be assigned an EMF maximum limit When the limit is exceeded the EMF flag in the user interface is displayed 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 Setting th
109. sition 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 Remove the pump head and examine the seals pistons and internal components for signs of wear contamination or damage Exchange components as required 2 Defective pump drive assembly Please contact your Agilent service representative Index Missing Index Missing Pump channel A B Index Missing Pump channel B The encoder index position in the module was not found during initialization 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 index position is not recognized within a defined time the error message is generated Probable cause Suggested actions 1 Disconnected or defective encoder cable Please contact your Agilent service representative 2 Defective pump drive assembly Please contact your Agilent service representative 1260 Capillary Pump User Manual Error Information 7 Stroke Length Stroke Length Pump channel A B Stroke Length Pump channel B The distance between the lower piston pos
110. ss I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards Operation 186 Before applying power comply with the installation section Additionally the following must be observed Do not remove instrument covers when operating Before the instrument is switched on all protective earth terminals extension cords auto transformers and devices connected to it must be connected to a protective earth via a ground socket Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury Whenever it is likely that the protection has been impaired the instrument must be made inoperative and be secured against any intended operation 1260 Capillary Pump User Manual Appendix 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 Any adjustment maintenance and repair of the opened instrument under voltage should be avoided whenever possible When inevitable this has to be carried out by a skilled person who is aware
111. ss the power plug gt Remove the power cable from the instrument before opening the cover gt Do not connect the power cable to the Instrument while the covers are removed 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 gt Notify your Agilent sales and service office about the damage gt An Agilent service representative will inspect the instrument at your site and initiate appropriate actions 1260 Capillary Pump User Manual 49 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 Status lamp Power switch Serial number Figure 11 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 The security lever will prevent that the cover is opened while the power cord is connected to the module 50 1260 Capillary Pump User Manual Installing the Module 3 Installing the Pump 5 Connect the required interface cables to the rear of the pump see Connecting Modules on page 52 Configuration switch Slot for interface board RS232 Remote Analog output C
112. sult 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 When the current reaches the maximum limit the module is switched off and the error message is generated Probable cause Suggested actions 1 Flow path blockage in front of the damper Ensure the capillaries and frits between the pump head and damper inlet are free from blockage 2 Blocked outlet valve Exchange the outlet valve 3 High friction partial mechanical blockage in Remove the pump head assembly Ensure there the pump drive assembly is no mechanical blockage of the pump head assembly or pump drive assembly 4 Defective pump drive assembly Please contact your Agilent service representative 5 Defective main board Please contact your Agilent service representative 6 Restriction capillary blocked at pre mixing Exchange restriction capillary union 1260 Capillary Pump User Manual 103 7 Error Information Encoder Missing Encoder Missing Pump channel A B Encoder Missing Pump channel B 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
113. systems te Agilent Technologies 61 4 Using the Pump Hints For Successfully Using the Pump 62 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 Always place the solvent cabinet with the solvent bottles on top or at a higher level of the pump Make sure the pump is only used with the provided stainless steel solvent filters Solvent inlet filter stainless steel p n 01018 60025 Glas inlet filters may release particles that impact the operation of the EMPV electromagnetic proportioning valve For the same reason never use the pump without filters Use the provided brown solvent bottle for aqueous solvents as the lower light transmission will help to prevent the growth of algae Clean the bottle regularly e g every second day and discard any unused solvent When using buffer solutions flush the system with water before switching it off Check the pump pistons for scratches when changing the piston seals Scratched pistons will lead to micro leaks and will decrease the lifetime of the seal After changing the piston seals apply the seal wear in procedure Place t
114. t 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 Hazard of electrical shock or damage of your instrumentation can result if the devices are connected to a line voltage higher than specified gt Connect your instrument to the specified line voltage only Module is partially energized when switched off as long as the power cord is plugged in Repair work at the module can lead to personal injuries e g electrical shock when the cover is opened and the module is connected to power gt Always unplug the power cable before opening the cover gt Do not connect the power cable to the instrument while the covers are removed CAUTION Unaccessable power plug In case of emergency it must be possible to disconnect the instrument from the power line at any time gt Make sure the power connector of the instrument can be easily reached and unplugged gt Provide sufficient space behind the power socket of the instrument to unplug the cable 34 1260 Capillary Pump User Manual Site Requirements and Specifications 2 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 ea
115. t performance A single injection of the Agilent Technologies isocratic test standard is made under the conditions given below Conditions Table 16 Conditions Flow Stoptime Solvent A Solvent B Wavelength DAD MWD Injector volume Column temperature Agilent 1260 Infinity Capillary LC Instrument Column Standard 15 0 pL min 7 00 min 30 HPLC grade water 70 HPLC grade acetonitrile Sample 254 4 nm reference 360 80 nm 200 nL 25 0 C or ambient 1260 Micro Degasser 1260 Capillary Pump 20 pL min sensor installed 1260 Micro High Performance Autosampler 1260 Thermostatted Column Compartment optional Detector 1260 Multiple Wavelength Detector VL or SL or 1260 Diode Array Detector VL or SL with 500 nL flow cell installed e Data system Column ZORBAX SB C18 5 um 150 x 0 5 mm p n 5064 8256 Agilent isocratic checkout sample p n 01080 68704 0 15 wt dimethylphthalate 0 15 wt diethylphthalate 0 01 wt biphenyl 0 03 wt o terphenyl in methanol Diluted 1 10 in acetonitrile For instrument configurations other than shown above the conditions are altered to match the specifications of the instrument 1260 Capillary Pump User Manual 67 4 Using the Pump Procedure 1 Make a single injection of the isocratic test standard under the conditions given below 2 Compare the resulting chromatogram with the typical chromatogram shown in Figure 15 on page 68
116. tenance and errors Housing All materials recyclable 1260 Capillary Pump User Manual 39 2 40 Site Requirements and Specifications Performance Specifications 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual 000 J e Go Installing the Module Unpacking the Module 42 Delivery Checklist 42 Capillary Pump Accessory Kit 43 Optimizing the Stack Configuration 44 One Stack Configuration 44 Two Stack Configuration 47 Installing the Pump 49 Connecting Modules and Control Software 52 Connecting Modules 52 Connecting a Vacuum Degasser 52 Connecting Control Software and or G4208 A Instant Pilot 53 Flow Connections 54 Get the System Ready for the First Injection 58 Manually Priming the Solvent Channels 58 Priming Your System With the Pump 59 This chapter provides information about the installation of the pump and the connection to other modules and to the control software ot Agilent Technologies m 3 Installing the Module Unpacking the Module CAUTION 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 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 gt
117. the light produced G by the deuterium lamp used in this product The apparatus is marked with this symbol when hot surfaces are available and the user should not touch it when heated up WARNING iia alerts you to situations that could cause physical injury or death gt Do not proceed beyond a warning until you have fully understood and met the indicated conditions CAUTION A CAUTION alerts you to situations that could cause loss of data or damage of equipment gt Do not proceed beyond a caution until you have fully understood and met the indicated conditions 188 1260 Capillary Pump User Manual Appendix 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 This product complies with the WEEE Directive 2002 96 EC marking requirements The affixed label indicates that you must not discard this electrical electronic product in domestic household waste Product Category With reference to the equipment types in the WEEE Directive Annex I this product is classed as a Monitoring and Control Instrumentation product s Do not dispose off in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com for m
118. the pump use the leak test see Leak Test Description on page 120 Step 2 When the system pressure reaches 390 bar the pump switches off The pressure drop from this point onwards should be no more than 2 bar min 1260 Capillary Pump User Manual Test Functions and Calibration 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 1260 Capillary Pump User Manual 117 8 Test Functions and Calibration Running the Pressure Test When Tools required Parts required Preparations 118 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 Wrench 1 4 inch p n Description 1 01080 83202 Blank nut 1 500 ml lsopropanol e Place a bottle of LC grade isopropanol in the solvent cabinet and connect it to channel A2 Install the manual purge valve from the accessories kit to pump head A Move the inline filter outlet capillary from the EMPV to to manual purge valve Make absolutely sure that all parts of the flow path that are part of the test are very thoroughl
119. tightened 1260 Capillary Pump User Manual 119 8 Test Functions and Calibration Leak Test Leak Test Description 120 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 After initialization pistons Al and B1 are both at the top of their stroke Next the pump begins pumping solvent with a flow rate of 150 uL min stroke of 100 uL and a composition of 51 A 49 B Both pumps deliver for one complete pump cycle At the end of this step pistons Al and B1 are at the top of their stroke Ramp 2 The pump continues pumping solvent with a flow rate of 150 uL min Channel A delivers for one pump cycle first piston A2 delivers then piston A1 followed by channel B piston B2 then piston B1 both channels with a stroke of 20 uL Ramp 3 Just before the start of the first plateau piston A2 delivers with a flow rate of 50 uL min for approximately 8 s Plateau 1 At plateau 1 piston A2 delivers with a flow rate of 3 uL min for 30 s Ramp 4 Piston B2 delivers 50 uL min for approximately 8 s 1260 Capillary Pump User Manual Test Functions and Calibration 8 Plateau 2 Piston B2 de
120. tons into the pump head assembly and press them completely into the seals Pump head assembly 4 Slide the pump head assembly onto the pump drive Apply a small amount of pump head grease to the pumphead screws and the balls of the spindle drive Tighten screws stepwise with increasing torque Balls of spindle drive Pump head screws _ 5 Reconnect the capillaries tubing and the active inlet valve cable to the connector AIV connector Adapter capillary pe Inlet tube Active inlet valve 1260 Capillary Pump User Manual 155 9 Maintenance 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 gt Be sure to hold the board by the edges and do not touch the electrical components Always use an ESD protection for example an ESD wrist strap when handling electronic boards and components _ Switch OFF the module at the main power switch Unplug the module from main power Disconnect cables from the interface board connectors Loosen the screws Slide out the interface board from the module Install the new interface board Secure the screws oa Ff O N Reconnect the ca
121. troduction to the 1260 Infinity Capillary Pump Table 2 Agilent 1200 Infinity Series Interfaces Module CAN LAN BCD LAN RS 232 Analog APG Special optional on board Remote G4212A B DAD 2 No Yes Yes 1 Yes G1315C DAD VL 2 No Yes Yes 2 Yes G1365C MWD G1315D DAD VL G1365D MWD VL G1321B FLD 2 Yes No Yes 1 Yes G1362A RID G4280A ELSD No No No Yes Yes Yes EXT Contact AUTOZERO Others G1316A C TCC 2 No No Yes No Yes G1322A DEG No No No No No Yes AUX G1379B DEG No No No Yes No No AUX G4227A Flex Cube 2 No No No No No G4240A CHIP CUBE 2 Yes No Yes No Yes CAN DC OUT for CAN slaves THERMOSTAT for G1330A B NOT USED 20 The detector DAD MWD FLD VWD RID is the preferred access point for control via LAN The inter module communication is done via CAN CAN connectors as interface to other modules LAN connector as interface to the control software e RS 232C as interface to a computer e REMOTE connector as interface to other Agilent products e Analog output connector s for signal output 1260 Capillary Pump User Manual Introduction to the 1260 Infinity Capillary Pump 1 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 G1
122. troduction to the 1260 Infinity Capillary Pump Electrical Connections Rear View of the Module Configuration switch Slot for interface board RS232 Remote Analog output CAN Bus Power Plug Security Lever Figure 3 Rear View of the Module NOTE The GPIB interface has been removed with the introduction of the 1260 Infinity modules 18 1260 Capillary Pump User Manual Interfaces Table 2 Agilent 1200 Infinity Series Interfaces Module CAN LAN BCD optional LAN on board Introduction to the 1260 Infinity Capillary Pump 1 RS 232 Analog The Agilent 1200 Infinity Series modules provide the following interfaces APG Special Remote Pumps G1310B Iso Pump G1311B Quat Pump G1311C Quat Pump VL G1312B Bin Pump G1312C Bin Pump VL 1376A Cap Pump G2226A Nano Pump G4220A B Bin Pump G1361A Prep Pump Samplers G1329B ALS G2260A Prep ALS G1364B FC PS G1364C FC AS G1364D FC uS G1367E HiP ALS G1377A HiP micro ALS G2258A DL ALS G4226A ALS Detectors G1314B VWD VL G1314C VWD VL G1314E F VWD Yes No Yes Yes Yes Yes Yes No No Yes No No No No No Yes Yes Yes Yes Yes Yes Yes Yes Yes No No No No No Yes Yes Yes CAN DC OUT for CAN slaves Yes THERMOSTAT for G1330B Yes THERMOSTAT for G1330B CAN DC OUT for CAN slaves Yes Yes Yes 1260 Capillary Pump User Manual 19 1 In
123. trument in an explosive atmosphere WARNING Electrical shock Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened gt Do not remove the metal top cover of the module No serviceable parts inside gt Only certified persons are authorized to carry out repairs inside the module WARNING Personal injury or damage to the product Agilent is not responsible for any damages caused in whole or in part by improper use of the products unauthorized alterations adjustments or modifications to the products failure to comply with procedures in Agilent product user guides or use of the products in violation of applicable laws rules or regulations gt Use your Agilent products only in the manner described in the Agilent product user guides CAUTION Safety standards for external equipment gt If you connect external equipment to the instrument make sure that you only use accessory units tested and approved according to the safety standards appropriate for the type of external equipment 1260 Capillary Pump User Manual 131 9 Maintenance Overview of Maintenance Table 24 Simple Repair Procedures Procedure Symptom Notes Removing the Active Inlet Valve on page 139 Exchanging the Outlet Valve Sieve on page 142 Exchanging the Solvent Selection Valve on page 144 Exchanging the Solvent Selection Valve on page 144
124. urring for both pump heads first determines the precise movement limits for both pistons These limits are then stored in the pump controller memory Then both pistons are set to their default initial positions When pumping begins the active inlet valve is opened and piston 1 begins its intake stroke sucking solvent into chamber 1 At the same time piston 2 begins its delivery stroke pumping high pressure the existing solvent in chamber 2 out of the pump head The pressure produced by piston 2 also 1260 Capillary Pump User Manual 11 1 introduction to the 1260 Infinity Capillary Pump Introduction to the Pump 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 The outlet valve is forced open by the pressure generated by piston 1 Piston 1 begins to deliver the volume previously sucked into chamber 1 Because of the 2 1 speed ratio of the pistons half of the solvent flow from chamber 1 is forced out of the pump head continuing into the pump hydraulic path The other half of the flow from chamber 1 simultaneously refills chamber 2 When piston 1 has completed its delivery stroke the pistons reverse direction
125. used for external contacts and BCD bottle number output or LAN connections The REMOTE connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features such as start stop common shut down prepare and so on e With the appropriate software the RS 232C connector may be used to control the module from a computer through a RS 232C connection This connector is activated and can be configured with the configuration switch e The power input socket accepts a line voltage of 100 240 VAC 10 witha line frequency of 50 or 60 Hz Maximum power consumption varies by module There is no voltage selector on your module because the power supply has wide ranging capability There are no externally accessible fuses because automatic electronic fuses are implemented in the power supply Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Serial Number Information ALL The serial number information on the instrument labels provide the following information CCXZZ00000 CC X ZZ 00000 1260 Capillary Pump User Manual Format Country of manufacturing DE Germany Alphabetic character A Z used by manufacturing Alpha numeric code 0 9 A Z where each combination unambiguously denotes a module there can be more than one code for the same module Serial number 17 1 in
126. ush the adapter onto the syringe 2 Fill required analytical solvents into the solvent bottles and install the bottles on the described solvent channels Use isopropanol for channels which will not be used right away 3 Put a paper towel over the leak sensor in the pump leak tray 4 Disconnect the channel A solvent tube from the A1 port of the pump solvent selection valve 5 Connect the end of the solvent tube to the syringe adapter Slowly draw one syringe volume 20 mL from the solvent tube 6 Disconnect the solvent tube from the syringe adapter and reconnect the tube to the A1 port of the solvent selection valve Eject the syringe contents into an appropriate waste container 1260 Capillary Pump User Manual Installing the Module 3 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 WARNING When opening capillary or tube fittings solvents may leak out The handling of toxic and hazardous solvents and reagents can bear health risks gt Please observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used At the pump activate t
127. valve in channel A 2 Loose pump head screws in channel A 3 Leaking seal or scratched piston in channel A2 Suggested actions Clean the outlet valve in channel A Ensure the sieve in the outlet valves are installed correctly Tighten the outlet valve Ensure the pump head screws in channel A are tight Exchange the pump seals in channel A Check the piston for scratches Exchange if scratched Second plateau negative or unstable and at least one other plateau positive Probable cause 1 Leaking outlet valve in channel B 2 Loose pump head screws in channel B 3 Leaking seal or scratched piston in channel B2 1260 Capillary Pump User Manual Suggested actions Clean the outlet valve in channel B Ensure the sieve in the outlet valves are installed correctly Tighten the outlet valve Ensure the pump head screws in channel B are tight Exchange the pump seals in channel B Check the piston for scratches Exchange if scratched 125 126 Test Functions and Calibration Third plateau negative or unstable and at least one other plateau positive Probable cause 1 Airin channel A or new seals not yet seated 2 Loose active inlet valve in channel A 3 Loose pump head screws in channel A 4 Loose outlet valve in channel A 5 Leaking seal or scratched piston in channel Al 6 Defective active inlet valve in channel A Suggested actions Flush channel A thoroughly with isopropanol under pressure use
128. vents described in Table 20 on page 79 If the solvent in use is not listed in the compressibility table when using premixed solvents and if the default settings are not sufficient for your application the following procedure can be used to optimize the compressibility settings Use the 1260 Capillary Pump in the Normal Mode at least 100 pL min 1 Start channel A of the pump with the adequate flow rate The system pressure must be between 50 and 250 bar 2 Before starting the optimization procedure the flow must be stable Use degassed solvent only Check the tightness of the system with the pressure test 3 Your pump must be connected to a data system or Instant Pilot with which the pressure and ripple can be monitored otherwhise connect a signal cable between the pressure output of the pump and a recording device for example 339X integrator and set parameters Zero 50 Att 2 3 Chart Speed 10 cm min 4 Start the recording device with the plot mode 1260 Capillary Pump User Manual Optimizing Performance 5 5 Starting with a compressibility setting of 10 x 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 78 through step 5 on page 79 for the B channel of your pump Table 20 Solvent Compressibility Solvent pure Compressibility 1
129. with 2 propanol or THF dissolve stainless steel Avoid the use of alkaline solutions pH gt 8 5 which attack the fused silica in PEEK coated fused silica capillaries 1260 Capillary Pump User Manual Using the Pump 4 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 Instrumental Problems Associated With Algae Algae deposit and grow everywhere within the HPLC system causing e Deposits on ball valves inlet or outlet resulting in unstable flow or total failure of the pump e Small pore solvent inlet filters to plug resulting in unstable flow or total failure of the pump Small pore high pressure solvent filters usually placed before the injector to plug resulting in high system pressure e Column filters to plug giving high system pressure e Flow cell windows of detectors to become dirty resulting in higher noise levels since the detector is the last module in the flow path this problem is less common Symptoms Observed with the Agilent 1260 Infinity HPLC The presence of algae in the Agilent 1260 Infinity can cause the
130. with homogenous solvent composition The flow rate for a nano pump is very low compared to the volume of the flow path Depending on the configuration it may take several hours to obtain stable conditions 1260 Capillary Pump User Manual 1260 Capillary Pump User Manual 5 Optimizing Performance Hints for the Micro Vacuum Degasser 74 Choosing the Right Pump Seals 75 How to Choose the Primary Flow 76 Static Mixer and Filter 77 How to Optimize the Compressibility Compensation Setting 78 This chapter provides additional information about further application specific hardware and parameter optimization te Agilent Technologies 73 5 Optimizing Performance 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 Capillary Pump at high flow rate 2 5 mL min Priming the degasser is recommended when e vacuum degasser is used for the first time or vacuum chambers are empty e changing to solvent that are immiscible with the solvent currently in the vacuum chambers e the pump was turned OFF for a length of time for example over night and volatile solvent mixtures are used For more information see Agilent 1260 Infinity G137
131. y flushed with isopropanol before starting to pressurize the system Any trace of other solvents or the smallest air bubble inside the flow path definitely will cause the test to fail Running the test from the Agilent Lab Advisor 1 Select the Pressure Test from the Test Selection menu 2 Start the test and follow the instructions Make sure to release the pressure by slowly opening the purge valve when the test has finished Evaluating the Results on page 119 describes the evaluation and interpretation of the Pressure Test results For detailed instructions refer to the Agilent Lab Advisor Software 1260 Capillary Pump User Manual Test Functions and Calibration 8 Evaluating the Results The sum of all leaks between the pump and the blank nut will be indicated by a pressure drop of gt 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 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 where not within the specified limits Often it is only a damaged blank nut itself poorly shaped from overtightening that causes a failure of the test Before investigating on any other possible sources of failure make sure that the blank nut you are using is in good condition and properly
132. yellow blinking modules without on board LAN indicator indicates that the module is in resident mode e g during update of main firmware A fast red blinking modules with on board LAN or fast yellow blinking modules without on board LAN indicator indicates that the module is in boot loader mode e g during update of main firmware In such a case try to re boot the module or try a cold start 1260 Capillary Pump User Manual 85 6 Troubleshooting and Diagnostics User Interfaces 86 Depending on the User Interface the available tests vary Some descriptions are only available in the Service Manual Table 21 Test Functions available vs User Interface Test Instant Pilot G4208A Agilent Lab Advisor software Micro Mode Pressure Test Yes Yes Normal Mode Pressure Test Yes Yes Leak Test Yes Yes EMPV Test No Yes EMPV Cleaning Yes Yes 1260 Capillary Pump User Manual Troubleshooting and Diagnostics 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 This includes diagnostic capabilities calibration procedures and maintenan
133. ystem make sure that the bench is designed to bear the weight of all modules The module should be operated in a horizontal position Condensation CAUTION Condensation within the module Condensation will damage the system electronics gt Do not store ship or use your module under conditions where temperature fluctuations could cause condensation within the module gt If your module was shipped in cold weather leave it in its box and allow it to warm slowly to room temperature to avoid condensation 36 1260 Capillary Pump User Manual Site Requirements and Specifications 2 Physical Specifications Table 13 Physical Specifications Type Specification Comments Weight 17 kg 38 Ibs Dimensions height x 180 x 345 x 435 mm 7 x 13 5 x 17 inches width x depth Line voltage 100 240 VAC 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 180 VA 75 W 256 BTU Maximum Ambient operating 4 to 55 C 41 to 131 F temperature Ambient non operating 40 70 C 4 158 F temperature Humidity lt 95 at 25 40 C 77 104 F Non condensing Operating Altitude Up to 2000 m 6562 ft Non operating altitude Up to 4600 m 15091 ft For storing the module Safety standards IEC CSA Installation Category II Pollution Degree 2 For indoor use only UL 1260 Capillary Pump User Manual 37 2 Site Requirements and Specifications Performance Specifications Table 14 Perform

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