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Agilent 1200 Infinity Series ELSD

1. Obtain an IP address automatically Use the following IP address IP address Subnet mask Default gateway Obtain DNS server address automatically Use the following DNS server addresses Preferred DNS server Alternate DNS server Validate settings upon exit Agilent 1200 Infinity Series ELSD User Manual 43 4 LAN Configuration PC and Agilent ChemStation Setup 3 Enter the following IP and subnet mask address for the PC IP address 192 168 254 1 Subnet mask 255 255 255 0 Internet Protocol Version 4 TCP IPv4 Properties i BRAUS heas Ls a x General Alternate Configuration settings below Automatic private IP address User configured Alternate DNS server Preferred WINS server Alternate WINS server W Validate settings if changed upon exit If this computer is used on more than one network enter the alternate IP IP address 192 168 254 Subnet mask 255 255 255 Default gateway Preferred DNS server 1 0 y ox cme 4 Click OK to save the configuration NOTE It can take several seconds for the alternative network settings to take effect 44 Agilent 1200 Infinity Series ELSD User Manual Agilent ChemStation Setup LAN Configuration PC and Agilent ChemStation Setup This procedure describes the Agilent OpenLAB ChemStati
2. si Telnet 156 141 59 43 ka a Figure 6 A connection to the module is made 3 Enter the following information when prompted login user Password Agilent The login details are case sensitive The password will be not visible on screen 4 At the gt prompt type set network to view the available commands l E Telnet 156 141 50 43 babe 40 Agilent 1200 Infinity Series ELSD User Manual LAN Configuration 4 Table5 Telnet commands Value Description set network displays syntax and descriptions of commands set network displays the current settings and list of commands set network ip lt x x x x gt sets new ip address set network submask lt x x x x gt sets new subnetmask set network gateway lt x x x x gt sets new default gateway set network static on off sets the ip to not change set network dhcp on off sets the device to or to not get its id from a dhcp server set network autoip on off sets the device to or tonot try to automatically get an ip quit closes telnet and disconnects you 5 To change a parameter follow the style Parameter value for example set network static on set network ip 156 141 59 43 Then press Enter Parameter refers to the configuration parameter you are defining and value refers to the definitions you are assigning to the parameter Each entry is followed by a carriage return 6 When you have finished typing the configuration parameters type quit and press Ent
3. Loading a Method To load one of the 10 on board methods highlight METHOD Using the arrow keys scroll up or down to the required method number The instrument will acknowledge the change by displaying the method number in the top left hand corner These on board methods cannot be edited Agilent 1200 Infinity Series ELSD User Manual 55 5 56 Using the Module Evaporator Temperature The evaporator temperature is the most important setting on the ELS detector This should be set according to the volatility of the compound s being analyzed If the compound is non volatile e g sugars then the evaporator temperature should be set to 80 90 C If the compound is semi volatile or has a low molecular weight e g pharmaceutical drug then the evaporator temperature should be set between 20 30 C The evaporator temperature ranges for the ELS models are as follows G4260B G4261B ELSD non cooled OFF 25 120 C 1 C increments G4261B ELSD cooled OFF 10 80 C 1 C increments The default evaporator temperature for both models is 30 C Nebuliser Temperature The nebuliser temperature can be used to optimize signal response in addition to evaporator temperature Higher nebuliser temperatures increase peak response but the nebuliser temperature must not exceed the boiling point of the mobile phase The nebuliser temperature range for both models is OFF 25 90 C 1 C increments The defa
4. 8 Ensure that the bottom of the waste tube is below the height of the waste outlet from the instrument Though it will not cause any damage if the solvent waste tube becomes submersed below the solvent level inside the waste container positive pressure will be exerted on the nebuliser chamber leading to excessive baseline noise 28 Agilent 1200 Infinity Series ELSD User Manual Installing the Module 3 WARNING Risk of intoxication and contamination of detector Toxic evaporation and accumulation of condensing solvent gt The exhaust must be extracted to a suitable fume extraction system gt Attach one end of the exhaust hose to the rear of the unit gt Ensure the exhaust hose has an upward slope from the detector so that any condensed solvent is collected in the waste bottle at the front of the unit and to prevent it accumulating in the tubing gt Make sure the other end of the exhaust hose is vented to a fume hood or other disposal unit 9 Connect the exhaust hose between the exhaust outlet and a fume hood 10 For digital data collection and control connect the LAN cable to the LAN interface OR Connect the RS232 serial cable 11 Connect the analog cable optional 12 Connect the injection trigger cable to the Agilent autosampler Analogue output cable Analogue output cable PL0890 0300 The ELS Detector is fitted with a LAN or standard RS232 3 wire serial interface Both connections provide a 24 bit80
5. 5 Using the Module LAN TCP IP Settings This screen displays the 1290 Infinity ELSD G4261B current configured TCP IP settings See LAN Configuration on page 33 for details on how too set these values Figure 10 TCP IP settings Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 Controlling the ELSD During an Injection The ELS Detector has the capability to change operational parameters in real time during a sample injection using an on board timetable Real time Operation The ELS Detector can store in memory a series of time based events within a single timetable This timetable allows the operational settings of the ELSD to be changed in real time during a run The evaporator temperature G4261B cooled gas flow PMT gain and smoothing parameters can all be configured within this timetable to change during a sample injection The timetable can be used to program the gas flow in order to compensate for the change in ELSD response across a solvent gradient Alternatively the timetable can be customized to create adjustable PMT gain across a sample injection for mixtures containing samples with wide concentration ranges The single timetable stored on board the ELSD is only customizable using the ELSD DIMENSION software which can be purchased from Agilent ELSD Dimension Software includes trigger cable PL0O890 0375 which also includes Trigger cable for Dimension Software Dimension t
6. 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 ESD protection for example an ESD wrist strap when handling electronic boards and components 100 Agilent 1200 Infinity Series ELSD User Manual Maintenance 9 Cleaning the Module The exterior of the instrument should be cleaned by wiping down with a soft cloth moistened with dilute detergent solution followed by wiping down with a cloth moistened with deionized water Ensure that no moisture enters the instrument WARNING Electrical shock and burns Liquid in the module electronics can cause shock hazard and damage the module gt Switch off and disconnect power cord from instrument before cleaning gt Do not use an excessively damp cloth during cleaning gt Drain all solvent lines before opening any fittings gt Allow the instrument to dry off completely before reconnecting power Agilent 1200 Infinity Series ELSD User Manual 101 9 Maintenance Inspection of Cables Periodically inspect the connecting cables for signs of physical damage caused by abrasion solvent spillage impact etc Replace damaged cables particularly the power cord if any damage is observed 102 Agilent 1200 Infinity Series ELSD User Manual Maintenance 9 Drying the Diffuser If the instrument has been operated incorrectly the diffuser may become blocked with liquid This is mani
7. a A 114 Agilent 1200 Infinity Series ELSD User Manual Appendix 11 A WARNING 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 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 Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards Agilent 1200 Infinity Series ELSD User Manual 115 11 Appendix Operation 116 Before applying power comply with the installation se
8. features Agilent 1200 Infinity Series ELSD User Manual 3 In This Book 8 Error Information This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions 9 Maintenance This chapter describes the maintenance of the ELSD 10 Parts and Materials for Maintenance This chapter provides information on parts for maintenance 11 Appendix This chapter provides addition information on safety legal and web 4 Agilent 1200 Infinity Series ELSD User Manual Contents Contents 1 Introduction to the Detector 7 Introductiontothe ELSD 8 System Overview 9 2 Site Requirements and Specifications 17 Pre installation Requirements 18 Site Requirements 19 Physical Specifications 22 Performance Specifications 23 3 Installing the Module 25 Unpacking the Module 26 Installing the Module 28 4 LAN Configuration 33 What You Have to Do First 34 TCP IP Parameter Configuration 35 PC and Agilent ChemStation Setup 42 5 Usingthe Module 47 Before Using the Detector 49 Instrument Controls 50 Operational Parameters 55 Controlling the ELSD During an Injection 61 Controlling the ELSD within ChemStation or EZChrom 64 General Considerations 65 Agilent 1200 Infinity Series ELSD User Manual Contents Optimizing Performance 69 Do s and Don ts of ELS Detection 70 Location of the Detector Module 71 Pumping systems 72 Mobile phase
9. 60 psi 2 Defective mass flow controller Please contact your Agilent service representative Agilent 1200 Infinity Series ELSD User Manual 91 8 Error Information Invalid Nebulizer temperature Error ID 22 Invalid nebulizer temperature reading Probable cause Suggested actions 1 Nebulizer heater not connected to the Please contact your Agilent service representative main board 2 Defective nebuliser heater Please contact your Agilent service representative Invalid Evaporator temperature Error ID 23 Invalid evaporator temperature reading Probable cause Suggested actions 1 Evaporator heater not connected to Please contact your Agilent service representative the main board 2 Defective evaporator heater Please contact your Agilent service representative Fan failed on cooled evaporator Error ID 24 Fans on cooled evaporator module have failed Probable cause Suggested actions 1 Fan not connected to peltier assembly Please contact your Agilent service representative 2 Defective peltier fan Please contact your Agilent service representative 92 Agilent 1200 Infinity Series ELSD User Manual Error Information 8 Cooled evaporator current out of range or communication failed Error ID 25 Peltier module current outside of normal range or communication to peltier module has failed Probable cause Suggested actions 1 Defective peltier assembly Please contact your Agilent service representative 2 Peltier as
10. Hz alternatively 40 or 10 Hz digital output for connection to a PC running a data acquisition package e g ChemStation software For further information on how to configure the PC with OpenLAB or ChemStation software refer to the appropriate user guide supplied with the driver install For further information on how to configure the TCP IP settings on the detector see LAN Configuration on page 33 Agilent 1200 Infinity Series ELSD User Manual 29 3 30 Installing the Module For digital data collection using ChemStation or EZChrom connect the ELS detector to the computer using the RS232 or LAN cable supplied with the detector The Injection Trigger Cable G4260 60005 is also required to start an injection and should be used to connect to the 1200 instrument remote connector The ELS Detector can be connected to auxiliary equipment such as an autosampler or pump via the 15pin remote start cable The remote start cable can be configured in several ways to allow on board timetable events to be triggered or to remotely auto zero The ELS detector is equipped with 2 contact closures normally open for stopping the operation of a pump if the unit reports an error condition Pump stop facility must be employed if the instrument is to be left unattended or if units are stacked The ELS Detector is also equipped with one contact closure which is normally open and two TTL logic inputs both active low with internal pull up re
11. Scattering Detector G4261B Agilent 1290 Infinity Evaporative Light Scattering Detector PL0880 0310 Analogue Cable PL0890 0305 Gas inlet tube 2 m PL0890 0310 Rear exhaust hose PVC 2 m PL0890 0315 Solvent waste tube 2 m PLO890 0325 RS232 communication cable PL0890 0345 Trigger Cable for Dimension Software PL0890 0350 Remote start cable third party LCs only G4260 90000 ELSD Operation Manual 112 Agilent 1200 Infinity Series ELSD User Manual Agilent 1200 Infinity Series ELSD User Manual 11 Appendix General Safety Information 114 The Waste Electrical and Electronic Equipment Directive 117 Radio Interference 118 Agilent Technologies on Internet 119 This chapter provides addition information on safety legal and web Ee Agilent Technologies 113 11 Appendix General Safety Information Safety Symbols Table 7 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to A the instruction manual in order to protect risk of harm to the operator and to protect the apparatus against damage Indicates dangerous voltages Indicates a protected ground terminal The apparatus is marked with this symbol when hot surfaces are available and the user should not touch it when heated up External Laser warning label located on rear of detector Internal Laser warning label located on light source Internal Laser beam label located on light source AN C
12. Series ELSD User Manual 2 Site Requirements and Specifications Pre installation Requirements 18 Site Requirements 19 Physical Specifications 22 Performance Specifications 23 This chapter provides information on environmental requirements physical and performance specifications ot Agilent Technologies 17 2 Site Requirements and Specifications Pre installation Requirements For a detailed description of the environmental and operating requirements of the ELSD please refer to the Site Preparation Checklist This manual will give you an overview of the ELS detector and describe its operation in more detail 18 Agilent 1200 Infinity Series ELSD User Manual Site Requirements and Specifications 2 Site Requirements A suitable environment is important to ensure optimal performance of the instrument please refer to the Site Preparation Checklist for more details Laser Safety The Agilent 1290 Infinity ELSD G4261B is classified as a Laser Class 1 product IEC825 1 CFR1040 10 amp 1040 11 During normal operation of the G4261B ELSD no laser light is accessible to the user WARNING Eye damage by laser light Hazardous laser light can injure eyes gt Do not remove covers and interlocks gt Observe and note the laser warning signs carefully Power Considerations Check the operating voltage of your instrument on the IEC inlet fuse holder on rear of unit WARNING Hazard of electrical shock or da
13. com 2 To login type the following information Username user Password Agilent The login details are case sensitive NOTE 9 Agilent 1200 Infinity Series ELSD User Manual 37 4 LAN Configuration TCP IP Parameter Configuration 3 From the left hand menu select Network to configure the TCP IP settings Agilent 1290 ELSD Configuration and Management e Network Configuration Configuration Spi Motwark Obtain an IP address automaticaly using DHCP Use the folowing IP address IP address Subnet Mask Default Gateway Changes to DHCP IP address and Subnet Mask require a reboot to take effect Apply b Network Servces Settings b Advanced Notwark Sethngs The detector can be configured to e obtain an IP address automatically DHCP use a static IP address change Hostname Advanced Network settings 4 To use a static IP address select Use the following IP address 5 Enter the module s IP Address Subnet Mask and Default Gateway address and click Apply e Nek Configuration v IP Settings Obtain an IP address automatically using DHCP Use the folowing IP address IP Address 156 141 59 43 Subnet Mask 255 255 255 128 Default Gateway 156 141 59 1 Changes to DHCP IP address and Subnet Mask require a reboot to take effect Lanoy gt Network Services Settings Advanced Network Settings Agilent Technologies Inc 2012 6 Select Apply again to confirm
14. flat baseline 80 82 Agilent 1200 Infinity Series ELSD User Manual frequency range 22 G gain 5 7 gas flow 5 7 H humidity 22 l inspecting cables 102 installation site requirements 17 instrument controls 50 instrument errors 54 instrument fails to zero 81 intensity light source 58 interactive menu bar 51 internal temperature exceeded lower imit 87 internal temperature exceeded upper imit 87 internet 119 introduction ELSD 8 invalid evaporator temperature 92 invalid nebulizer temperature 92 K keypad 50 L LAN interface 34 LAN TCP IP parameter configuration 35 large baseline offset 81 laser current out of range 93 aser interlock open or failed 94 aser safety 19 aser temperature out of range 93 eak detected 89 eak sensor failed 95 LED light source error 91 LED 58 ine frequency 22 ine voltage 22 ocation detector 71 ow sensitivity 79 M MAC address 34 main menu bar 51 materials identifying 112 method 55 loading 55 nebulization 9 nebulizer temperature limit exceeded 90 no power 82 no response 82 non operating altitude 22 non operating temperature 22 0 on board vapor sensor failed 88 operating Altitude 22 operating temperature 22 operation principle detection 10 evaporation 9 nebulization 9 operational parameters 12 Agilent 1200 Infinity Series ELSD User Manual Index operation realtime 61 overview of detector 13 P packaging damaged 26 parts damaged 27 iden
15. in minutes at the top centre of the ELSD display When the timetable reaches the end of its run time the ELSD will revert to RUN mode and be primed ready to start the timetable again During an active timetable where the evaporator temperature is being controlled the status of the instrument will change from READY to NOT READY This is normal behavior and will not affect the running of the timetable Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 Figure 11 ELSD front panel display during timetable operation 1 Current runtime 2 Total runtime 3 On board Timetable is active The STOP button on the instrument s front keypad can be used to interrupt the active timetable whilst it is running When the STOP button is pressed the instrument will revert to STANDBY mode Agilent 1200 Infinity Series ELSD User Manual 63 5 Using the Module Controlling the ELSD within ChemStation or EZChrom The ELS Detector can be controlled directly using OpenLAB ChemStation and EZChrom editions and ChemStation Rev B 04 03 Digital data acquisition is performed without the need for an A D interface Controlling the ELSD using OpenLAB provides full detector functionality with the added benefit of remote automation The ELSD Driver is supplied on the CD supplied with the detector For further information on how to install and configure the ELSD driver refer to the appropriate user guide supplied with the driver install T
16. mode Should the instrument default to STANDBY mode the gas will reduce to a default value of 1 2 SLM for 15 min before closing Agilent 1200 Infinity Series ELSD User Manual Introduction to the Detector 1 Overview of ELS Detector Figure 3 ELSD overview front 1 Front screen display 2 Keypad 3 Eluent inlet 4 Solvent waste outlet Agilent 1200 Infinity Series ELSD User Manual 13 1 Introduction to the Detector Figure 4 ELSD overview rear 1 Vapour Sensor vent 2 Serial RS232 port 3 LAN connector only active on G4261B ELSD 4 Firmware button 5 1 0 connector Remote Start input 6 Mains Switch 7 Mains Input 8 Fuses 9 Gas inlet port 10 Exhaust port 11 Analogue Output 14 Agilent 1200 Infinity Series ELSD User Manual Introduction to the Detector 1 Table 1 ELS Detector 1 0 connections 1 0 description Pin number Inputs Timetable Start 14 amp ground Injection Sync 13 amp ground Remote A Z 7 amp ground Output Pump stop contact closure 3 amp 10 normally open Ground to case 1 5 6 11 In order to make appropriate remote start and A Z connections from a third party LC a Remote Start Cable Remote start cable third party LCs only PL0890 0350 can be purchased from Agilent Technologies Agilent 1200 Infinity Series ELSD User Manual 15 1 Introduction to the Detector System Overview 16 Agilent 1200 Infinity Series ELSD User Manual Agilent 1200 Infinity
17. outlet gt NEVER allow the solvent waste outlet tube to become immersed in the waste solvent gt When placing more than one HPLC detector in series always place the ELS detector last gt Only use volatile mobile phase additives 70 Agilent 1200 Infinity Series ELSD User Manual Optimizing Performance 6 Location of the Detector Module Place the detector conveniently near your HPLC system The modular design of the ELSD enables you to locate it anywhere within the limitations imposed by the length of the power cord fluid lines and signal cables In order to keep liquid dead volume as low as possible and to minimize peak broadening in the lines the distance between the column outlet and the flow cell inlet should be kept to a minimum Provide approximately four inches 10 cm of space behind the unit so that the cooling fan intake is not impeded and to allow easy access to the rear panel The ELS detector can be placed within 2 meters of an extraction unit using the exhaust tube provided Agilent 1200 Infinity Series ELSD User Manual 71 Optimizing Performance Pumping systems 72 It is recommended to use a high performance pumping system with no flow pulses to minimize nebulization problems Inconsistent solvent flow will result in poor reproducibility A backpressure regulator maybe necessary on certain pumps in order to minimize pulsation This can also be achieved by the column itself or a coil of 0 127 m
18. powered on Probable cause Suggested actions 1 Temperature probe fault or disconnected Check RTD connections Consult Agilent Technologies or your local agent for further advice Display not on but power connected Probable cause Suggested actions 1 Instrument Power Supply Refer to local distributor or Agilent Technologies 2 Faulty display Refer to local distributor or Agilent Technologies Evaporator Temperature reads zero at start up and cannot be changed Probable cause Suggested actions 1 Peltier cooler has not initiated correctly Switch detector off then on at the power socket Consult Agilent Technologies or your local agent if problem persists Agilent 1200 Infinity Series ELSD User Manual 83 7 84 Troubleshooting and Diagnostics Vapor sensor error occurs but there is no solvent or vapor leak inside unit Probable cause Suggested actions 1 Solvent vapor near the front of unit is being Remove any solvent bottle or solvent leak that drawn into the unit is directly in front of the detector 2 Faulty Vapor sensor Check the rear vapor sensor is not damaged bent Cooled Evaporator will not reach low temperature e g 10 C Probable cause Suggested actions 1 Ambient lab temperature too high Move detector to laboratory where ambient temperature is lt 25 C 2 Faulty Peltier cooler unit Consult Agilent Technologies or your local agent if problem persists Agilent 1200 Infinity Series ELSD User M
19. priming 73 Solvent recommendations 74 Troubleshooting and Diagnostics 75 Troubleshooting 76 Troubleshooting an HPLC System 77 General Problems 78 Error Information 85 What Are Error Messages 86 Module Specific Error Messages 87 Maintenance 97 Introduction to Maintenance 98 Cautions and Warnings 99 Cleaning the Module 101 Inspection of Cables 102 Drying the Diffuser 103 Cleaning Evaporator Tube 104 Putting the Instrument into Storage 105 Replacing Detector Firmware 106 10 Parts and Materials for Maintenance 111 Identifying Parts and Materials 112 11 Appendix 113 General Safety Information 114 The Waste Electrical and Electronic Equipment Directive 117 Radio Interference 118 Agilent Technologies on Internet 119 Agilent 1200 Infinity Series ELSD User Manual a Agilent 1200 Infinity Series ELSD User Manual KP e o e e00 ee 1 7 e Introduction to the Detector amp e e e Introduction to the ELSD 8 System Overview 9 Basic Principles of Operation Operational Parameters Overview of ELS Detector 9 12 13 This chapter gives an introduction to the module instrument overview and internal connectors if Agilent Technologies 1 Introduction to the Detector Introduction to the ELSD The Evaporative Light Scattering Detector is a unique and highly sensitive detector for semi volatile and non volatile solutes in a liquid stream It is mainly used as a concentration detector for High Pe
20. service representative 3 Defective main board Please contact your Agilent service representative Agilent 1200 Infinity Series ELSD User Manual Error Information 8 Leak Sensor failed Error ID 30 The leak sensor in the module has failed Probable cause Suggested actions 1 Leak sensor not connected to the main Please contact your Agilent service board representative 2 Defective leak sensor Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative Agilent 1200 Infinity Series ELSD User Manual 95 8 Error Information Module Specific Error Messages 96 Agilent 1200 Infinity Series ELSD User Manual Agilent 1200 Infinity Series ELSD User Manual 9 Maintenance Introduction to Maintenance 98 Cautions and Warnings 99 Cleaning the Module 101 Inspection of Cables 102 Drying the Diffuser 103 Cleaning Evaporator Tube 104 Putting the Instrument into Storage 105 Replacing Detector Firmware 106 This chapter describes the maintenance of the ELSD ee Agilent Technologies 97 9 Maintenance Introduction to Maintenance Trained personnel only should carry out maintenance inside the unit There are no user serviceable parts inside the instrument Unauthorized access to the instrument will invalidate the instrument warranty 98 Agilent 1200 Infinity Series ELSD User Manual Maintenance 9 Cautions and Warnings Toxic flammable and hazardous
21. solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks gt When working with these substances observe appropriate safety procedures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice gt The volume of substances should be reduced to the minimum required for the analysis gt Do not operate the instrument in an explosive atmosphere 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 cover of the module gt Only certified persons are authorized to carry out repairs inside the module Eye discomfort The light source in the G4260B ELSD is a Class 1 LED product Temporary discomfort may result from directly viewing the light produced by this source gt Do not look into the beam Agilent 1200 Infinity Series ELSD User Manual 99 9 Maintenance WARNING Fire and damage to the module Wrong fuses gt Make sure that only fuses with the required rated current and of the specified type super fast fast time delay etc are used for replacement gt The use of repaired fuses and the short circuiting of fuse holders must be avoided CAUTION Electronic boards and components are sensitive to electrostatic discharge ESD
22. the Agilent 1290 Infinity Evaporative Light Scattering Detector G4261B The manual describes the following e Introduction e Site Requirements and Specifications Installation e LAN Configuration e Using Optimizing e Troubleshooting and Diagnostics e Error Information Maintenance e Parts e Safety Agilent Technologies 2012 Printed in Germany 10 2012 G4260 90001 EE Agilent Technologies
23. 8 Baseline spikes 79 Low sensitivity and baseline noise drift 79 Spiky peak tops but flat baseline 80 Large Baseline offset 81 Peak tailing 81 Instrument Fails to zero 81 No power 82 No response completely flat baseline 82 Temperature error as soon as instrument powered on 83 Display not on but power connected 83 Evaporator Temperature reads zero at start up and cannot be changed 83 Vapor sensor error occurs but there is no solvent or vapor leak inside unit 84 Cooled Evaporator will not reach low temperature e g 10 C 84 This chapter gives an overview about the troubleshooting and diagnostic features oh Agilent Technologies 75 7 Troubleshooting and Diagnostics Troubleshooting 76 If a problem is encountered Agilent Technologies advises that the troubleshooting section should be followed first to resolve the problem If there is an error or fault and you follow the recommended course of action and the result is not satisfactory then please direct the matter to Agilent Technologies or your local distributor Malfunctions within the ELS Detector can arise from three general sources The ELS Detector itself can be dirty or operating outside specification The HPLC system can have a broken dirty or non optimally operating component but the problem is manifesting itself in the ELS Detector e A mobile phase and or column problem which by its very nature is spread throughout the HPLC system but appea
24. Control address for further reference The MAC or hardware address of the LAN interface is a worldwide unique identifier No other network device will have the same hardware address The MAC address can be found at detector start up see Configuration Using Instrument Front Panel on page 36 2 Connect the instrument s LAN interface to the PC network card using a crossover network cable point to point or a hub switch using a standard LAN cable Agilent 1200 Infinity Series ELSD User Manual LAN Configuration 4 TCP IP Parameter Configuration To operate properly in a network environment the LAN interface must be configured with valid TCP IP network parameters There parameters are e IP address e Subnet Mask Default Gateway The TCP IP parameters can be configured by the following methods e by manually setting the parameters via the front panel of the detector by manually setting the parameters through the G4261B ELSD web interface e by manually setting the parameters through a Telnet session The module can be configured via the front panel to obtain an IP address automatically or to use a static IP address see Table 4 on page 35 When configured to obtain its IP address automatically the module will request an IP address from the DHCP server after every power cycle If the detector is assigned a temporary IP address e g DHCP server then communication with the PC may be prevented following a power cycle o
25. a oe ewe aan Agilent Technologies Notices Agilent Technologies Inc 2012 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 64260 90001 Edition 10 2012 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn This product may be used as a com ponent of an in vitro diagnostic sys tem if the system is registered with the appropriate authorities and com plies with the relevant regulations Otherwise it is intended only for gen eral laboratory use Warranty The material contained in this docu ment is provided as is and is sub ject to being changed without notice in future editions Further to the max imum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or perfor mance of this document or of any information contained herein Should Agilent and the user
26. acking the Module 26 Installing the Module 28 Connecting the Detector to your LC System 28 Checking Operation of the ELS Detector 31 This chapter gives information about the installation of your ELSD i Agilent Technologies 25 3 Installing the Module Unpacking the Module Damaged Packaging If the delivery packaging shows signs of external damage please call your Agilent Technologies sales and service office immediately Inform your service representative that the instrument may have been damaged during shipment CAUTION Defective on arrival problems If there are signs of damage please do not attempt to install the module Inspection by Agilent is required to evaluate if the instrument is in good condition or damaged 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 26 Agilent 1200 Infinity Series ELSD User Manual Delivery Checklist Installing the Module 3 Unpack the ELSD and accessories and ensure that all parts and materials shown in the table below have been delivered with your module Report any missing or damaged parts to your local Agilent Technologies sales and service office p n Description G4260B OR G4261B PL0890 0355 PL0890 0325 8121 0008 G4260 60005 PL0890 0305 PL0890 0310 G4261 63000 N A N A Agilent 1200 Infinity Series ELSD User Manual Agi
27. ait 1h 79 7 Troubleshooting and Diagnostics Spiky peak tops but flat baseline Probable cause Suggested actions 1 Inconsistent nebulization Nitrogen is the recommended gas others can be used but may not nebulize as efficiently 2 Incorrect gas being used Change gas to nitrogen or evaluate different nitrogen sources 3 Poor regulation of inlet gases e Ifusing bottled gas check that gas regulator is functioning correctly and giving consistent flow e Alternatively use a pulse dampener 4 Insufficient smoothing The broader the peaks the higher the smoothing value is required Increase smoothing to 50 for Flash separations 5 Sample precipitation during nebulization Reduce sample concentration or inject same loading in larger volume Check sample solubility in mobile phase eluents 6 Inconsistent pump flow rates See remedy for pump pulsation in the baseline noise section 80 Agilent 1200 Infinity Series ELSD User Manual Large Baseline offset Probable cause 1 Inefficient evaporation 2 High concentration of non volatile buffer or stabiliser 3 Contaminated diffuser 4 Optics Heater failed Peak tailing Probable cause 1 Eluent particles lingering in the optical chamber 2 Poor chromatography Instrument Fails to zero Probable cause 1 Offset too high or output unstable due to impurity in mobile phase Agilent 1200 Infinity Series ELSD User Manual Troubleshooting and Diagnostics 7 Suggested acti
28. anual Agilent 1200 Infinity Series ELSD User Manual 7 e Error Information e What Are Error Messages 86 Module Specific Error Messages 87 Internal temperature exceeded lower limit 87 Internal temperature exceeded upper limit 87 On board Vapor sensor failed 88 Rear Vapor sensor failed 88 Vapor detected 88 Leak detected 89 Fan Failed 89 Fan Stopped 90 Nebulizer temperature limit exceeded 90 Evaporator temperature limit exceeded 91 LED light source error 91 Evaporator gas flow rate limit exceeded 91 Invalid Nebulizer temperature 92 Invalid Evaporator temperature 92 Fan failed on cooled evaporator 92 Cooled evaporator current out of range or communication failed 93 Laser temperature out of range 93 Laser current out ofrange 93 Laser interlock open or failed 94 Communication to Laser failed 94 Leak Sensor failed 95 This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions Apg Agilent Technologies 85 8 Error Information 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 t
29. ases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or make any unauthorized modification to the instrument Capacitors inside the instrument may still be charged even though the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious personal injury are present in this instrument Use extreme caution when handling testing and adjusting When working with solvents observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used Agilent 1200 Infinity Series ELSD User Manual Appendix 11 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 Ins
30. ative importance of refraction and reflection can be understood by examining the effects of the incident light on a single spherical particle whose equilateral axis lies in the same plane as the photodetector and light source With this configuration refraction is of greater significance than reflection The majority of organic compounds have refractive indices between 1 3 and 1 5 Changes in the refractive index within this range will not greatly affect the quantity of light reaching the detector This accounts for similarities in the sensitivity of the instrument to various compounds Agilent 1200 Infinity Series ELSD User Manual 11 1 12 Introduction to the Detector Operational Parameters The ELS Detector responds to all compounds that are less volatile than the mobile phase and is independent of a compound s optical properties It therefore provides advantages over other spectroscopic detectors for detecting compounds that are deficient in a UV chromophore or fluorophore The removal of aqueous mobile phase within an ELSD is typically achieved by setting the evaporator temperature to the eluent s boiling point e g 100 C in order to remove the solvent For non volatile compounds operating at these high temperatures maximizes the signal response However at these temperatures volatile and semi volatile compounds are destroyed and are therefore not detected This is problematic for small molecules such as pharmaceuticals an
31. ature 56 Evaporator Gas Flow 57 Detector Gain PMT 57 Response Time Smoothing 58 Light Source Intensity LED 58 Power Mode 59 Data Output Rate Hz 59 LAN TCP IP Settings 60 Controlling the ELSD During an Injection 61 Real time Operation 61 Creating a Real time Program 62 Starting and Stopping Real time Control 62 Controlling the ELSD within ChemStation or EZChrom 64 General Considerations 65 Solvent Recommendations 66 Sample Preparation 66 agigi Agilent Technologies 41 5 48 Using the Module Column Considerations 66 Transferring ELSD Temperature Methods 68 This chapter explains the operational parameters of the ELSD Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 Before Using the Detector On start up of the Agilent 1290 Infinity ELSD G4261B either Serial or LAN must be selected as the method of communication If Serial communication is selected then no further configuration is required The Agilent 1260 Infinity ELSD G4260B can only be connected through Serial communication When LAN communication is selected further configuration of the network settings is required see LAN Configuration on page 33 The Agilent 1260 Infinity ELSD does not have LAN communication functionality Agilent 1200 Infinity Series ELSD User Manual 49 5 Using the Module Instrument Controls 50 The ELS Detector can be used as a standalone detector via the front keypad and screen as sho
32. ay address use the up down arrow keys 9 When all values are populated press AZ Stop to accept The instrument will return an INVALID network setting message if the IP address and Gateway combination are incompatible The instrument will continue to the main menu screen to confirm the settings have been implemented Once the LAN settings are configured they are stored in memory even after a power cycle The MAC address and Host Names of the instrument are displayed on the LAN configuration screens for reference Agilent 1200 Infinity Series ELSD User Manual LAN Configuration 4 TCP IP Parameter Configuration Configuration Using Web Browser This procedure describes how to change the TCP IP parameters and hostname using a PC via a web browser 1 Using a web browser such as Internet Explorer type in the Host name or IP address of the ELSD into the address bar for example http 192 168 254 27 NOTE The default host name is configured to the detector s serial number If communication is successful the following login screen will appear rete Agilent 1290 ELSD Configuration and Management Welcome to the Configuration and Management interface of the Agilent Usemame s20 ASD Password Please specify the usemame and password to login to the web interface See the User Guide and documentation for more information on logging Logn in or retrieving a lost password Agilent Technologies inc 2012 www salent
33. clean and dry 3 If the baseline noise is within the limits autozero the detector However if the baseline noise is outside the limits refer to the Troubleshooting section for steps to rectify this Baseline noise should not have increased significantly and should be 0 5 mV Typically pure water should give no more than 0 4 mV peak peak whilst pure organic solvents should be less than 0 3 mV 4 Turn on the eluent flow and allow the system to stabilize 5 Again check the baseline noise Where noise and all other conditions are acceptable the instrument is ready to begin work Some volatile buffers can generate considerable offsets and increased noise levels Agilent 1200 Infinity Series ELSD User Manual 31 3 Installing the Module Installing the Module 32 Agilent 1200 Infinity Series ELSD User Manual Agilent 1200 Infinity Series ELSD User Manual 4 LAN Configuration What You Have to Do First 34 TCP IP Parameter Configuration 35 Configuration Using Instrument Front Panel 36 Configuration Using Web Browser 37 With Telnet 39 PC and Agilent ChemStation Setup 42 PC Setup for Local Configuration 42 Agilent ChemStation Setup 45 This chapter provides information on connecting the module to the controller software Ee Agilent Technologies 33 4 LAN Configuration What You Have to Do First 34 The Agilent 1290 Infinity ELSD G4261B has an on board LAN communication interface 1 Note the MAC Media Access
34. could result in damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated condi tions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indi cated conditions are fully under stood and met Agilent 1200 Infinity Series ELSD User Manual In This Book In This Book This manual contains information on e Agilent 1260 Infinity ELSD G4260B e Agilent 1290 Infinity ELSD G4261B 1 Introduction to the Detector This chapter gives an introduction to the module instrument overview and internal connectors 2 Site Requirements and Specifications This chapter provides information on environmental requirements physical and performance specifications 3 Installing the Module This chapter gives information about the installation of your ELSD 4 LAN Configuration This chapter provides information on connecting the module to the controller software 5 Using the Module This chapter explains the operational parameters of the ELSD 6 Optimizing Performance This chapter gives hints on how to optimize the performance or use additional devices 7 Troubleshooting and Diagnostics This chapter gives an overview about the troubleshooting and diagnostic
35. ction 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 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 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 g
36. ctionality and compliance with safety or EMC regulations 20 Agilent 1200 Infinity Series ELSD User Manual Site Requirements and Specifications 2 WARNING 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 Agilent 1200 Infinity Series ELSD User Manual 21 2 Site Requirements and Specifications Physical Specifications 22 Table 2 Physical Specifications Type Specification Comments Weight 11 kg G4260A 13 kg G4261A Dimensions 415 x 200 x 450 mm height x width x depth Line voltage Line frequency Power consumption Ambient operating temperature Ambient non operating temperature Humidity Operating altitude Non operating altitude Safety standards IEC CSA UL 16 3 x 7 9 x 17 7 inches 100 120 VAC or 220 240 V 10 50 or 60 Hz 5 150 W max Maximum 10 35 C 50 95 F 40 70 C 4 158 F lt 95 at 25 40 C 77 104 F Non condensing 80 at 31 C 88 F 50 at 40 C 104 F Up to 2000 m 6562 ft Up to 4600 m 15091 ft For storing the module Installation category II Pollution degree2 For indoor use only Agilent 1200 Infinity Series ELSD User Manual Performance Specifications Site Requirements and Specifica
37. d drug candidates The ELS detectors are specifically designed to evaporate difficult solvents at ambient and sub temperatures in order to maximize detection of semi volatile compounds The ELSD has patented technology that reduces the evaporation time of highly aqueous solvents at low temperature and also prevents the evaporation tube becoming saturated which would otherwise prevent further evaporation occurring Using this patented evaporation gas technology a 20 um droplet of water at 30 C can be dried ca 3x faster than just temperature alone Using the Agilent 1290 Infinity ELSD G4261B water can be evaporated as low as 20 C providing maximum sensitivity to thermally sensitive compounds For maximum sensitivity of non volatile compounds the evaporation gas can be turned off at higher evaporation temperatures Therefore unlike other ELS detectors where the evaporator temperature is set according to the type of mobile phase the ELS detector evaporator temperature is independent of the mobile phase Consequently the ELS detector can be set at 30 C for all types of mobile phase provided the evaporator gas flow is adjusted accordingly This method of operation ensures that the ELSD sensitivity is maximized even for low molecular weight compounds To prevent against unnecessary gas usage a controlled gas shut off valve is integrated into the detector gas manifold This will only allow gas to pass into the instrument when in RUN
38. ddress r Agilent 1290 Infinity ELSD 642618 Configuration aa Agilent 1290 Infinity ELSD RC NET Driver Communication Device name ELSD Type ID G4261Bnon cooled v Serial number COM port 16 J IP Address 156 141 59 120 Hostname L OK Cancel Help E 4 OR Select Hostname and enter the instrument s serial number Agilent 1290 Infinity ELSD 642618 Configuration s Agilent 1290 Infinity ELSD RC NET Driver Communication Device name ELSD j Serial number COMpot 16 IP Address 156 141 59 120 Hostname GB12080001 OK Cancel Help L 4 5 Select OK to complete the configuration NOTE The detector s serial number is the default hostname NOTE If the detector is assigned a temporary IP address e g DHCP server then communication with ChemStation maybe be prevented following a power cycle of the instrument Recommend using a static IP address to ensure communication with ChemStation is preserved after power cycle 46 Agilent 1200 Infinity Series ELSD User Manual Agilent 1200 Infinity Series ELSD User Manual 5 Using the Module Before Using the Detector 49 Instrument Controls 50 Display Screen 50 Keypad 50 Main menu bar 51 Sub Menu Screen 51 Status Mode 53 Error conditions 54 Clearing an Error 54 Operational Parameters 55 Method 55 Evaporator Temperature 56 Nebuliser Temper
39. enu Screen The sub menu screen is accessed from the front screen by selecting the key This screen allows changes to the following electronic parameters PMT Set Signal Gain SMTH Set Time Constant LED Set Light Source Intensity G4260B only PWR MODE Set Mode of ELSD when powered up HZ Set Data Output Rate LAN Displays the Instruments TCP IP settings G4261B only Agilent 1200 Infinity Series ELSD User Manual 51 5 Using the Module Figure 9 G4260B sub menu screen 52 Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 Status Mode CAUTION The ELS Detector can be operated in two modes STANDBY or RUN both of which are described over page To display the current mode and or select a new mode highlight the MODE function on the instrument display The current mode will now be displayed on the screen Using the arrow keys scroll up or down until the desired option is displayed The instrument acknowledges the command by displaying the mode of operation in the top right hand corner of the screen Standby The STANDBY mode is the ground state of the ELS detector which is by default initiated automatically after power on default can be changed using Power Mode Power Mode on page 59 In STANDBY mode the heaters and light source are switched off and the gas manifold valve is closed at power on The STANDBY mode gives the user a control platform in which to set up the operational param
40. er to exit 7 Restart the module for the new TCP IP settings to be implemented Agilent 1200 Infinity Series ELSD User Manual 41 4 LAN Configuration PC and Agilent ChemStation Setup 42 PC Setup for Local Configuration This procedure describes how to the change the TCP IP settings on your PC to match the modules default parameters in a local configuration using a cross over LAN cable see Table 4 on page 35 1 Open the Local Area Connection Properties and select Internet Protocol TCP IP Then click on Properties 4 Local Area Connection Properties x Networking Authentication Sharing Connect using i Intel R 82567LM Gigabit Network Connection Configure This connection uses the following items M Client for Microsoft Networks a M VMware Bridge Protocol M fE QoS Packet Scheduler 4 M 8 File and Printer Sharing for Microsoft Networks Intemet Protocol TCP IP E m Install Uninstall Description Allows your computer to access resources on a Microsoft network OK Cancel Agilent 1200 Infinity Series ELSD User Manual LAN Configuration 4 PC and Agilent ChemStation Setup 2 Select Alternative Configuration Internet Protocol Version 4 TCP IPv4 Properties You can get IP settings assigned automatically if your network supports this capability Otherwise you need to ask your network administrator for the appropriate IP settings
41. esentative 3 Defective main board Please contact your Agilent service representative Nebulizer temperature limit exceeded Error ID 18 Nebuliser temperature exceeded threshold after stabilizing Probable cause Suggested actions 1 Defective thermocouple Please contact your Agilent service representative 2 Defective nebuliser heater Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative 90 Agilent 1200 Infinity Series ELSD User Manual Error Information 8 Evaporator temperature limit exceeded Error ID 19 Evaporator temperature exceeded threshold after stabilizing Probable cause Suggested actions 1 Defective thermocouple Please contact your Agilent service representative 2 Defective evaporator heater assembly Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative LED light source error Error ID 20 The LED light source has failed Probable cause Suggested actions 1 LED Light source not connected to the Please contact your Agilent service representative main board 2 Defective LED Light source Please contact your Agilent service representative Evaporator gas flow rate limit exceeded Error ID 21 Evaporator gas flow rate exceeded threshold after stabilizing Probable cause Suggested actions 1 Insufficient gas inlet pressure Ensure the gas inlet pressure is above
42. eters gas flow nebuliser and evaporator temperatures before switching the unit into RUN mode The instrument will default to STANDBY mode should an error occur on the instrument When the instrument is switched from RUN mode to STANDBY mode following a command or error then the gas management system is invoked and the gas flow set to a minimum flow of 1 2 SLM for 15 min before the gas manifold valve is closed This minimum blanket gas is enough to nebulise and evacuate solvent should the instrument default to STANDBY mode with solvent still flowing Flooding the detector If the instrument is left in Standby mode for longer than 15 minutes gas flow to the unit is stopped to minimize gas usage gt The solvent pump must be turned off if the ELSD is going to be left in Standby mode longer than 15 minutes to prevent solvent flooding the detector RUN The RUN mode is the detector s operational mode In this mode the instrument is controlled at the set temperatures and gas flow and the system is fully operational During heating or cooling the instrument will display NOT READY to show the system has not reached the set conditions When the instrument has equilibrated READY will be displayed and the instrument is ready for use Agilent 1200 Infinity Series ELSD User Manual 53 5 Using the Module Error conditions The ELS Detector is equipped with a number of sensors and error checking facilities to ensure safe operation I
43. f an error is detected the instrument gives an audible warning and a visible description of the error condition In event of any error condition the unit defaults into the STANDBY mode in which the heaters light source and gas are turned off A complete list of instrument errors and remedial actions are given in the troubleshooting section of this manual CAUTION Solvent flooding the detector gt Itis strongly recommended that the pump stop from the 1 0 connector of the ELSD is connected to the HPLC pump to prevent solvent flooding the detector should an error occur Clearing an Error Once the source of the problem has been corrected select RUN mode to put the ELSD back into its operational state If the problem has not been rectified the ELSD will repeatedly error when RUN mode is selected 54 Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 Operational Parameters Method The ELS Detector has 10 on board pre set methods These methods comprise evaporator and nebuliser temperature and gas flow which can be optimized for specific applications These 10 on board methods are selected using the front keypad and screen via the METHOD option In addition to the 10 on board pre set methods the ELS Detector has a method XXX that allows modification of the ELSD parameters to be made without the need for software control Method XXX allows the detector to be used in standalone mode via the front screen and keypad
44. f the instrument Table4 Default STATIC IP parameters IP address 192 168 254 27 Subnet Mask 255 255 255 0 Default Gateway 192 168 254 1 Agilent 1200 Infinity Series ELSD User Manual 35 4 36 LAN Configuration Configuration Using Instrument Front Panel Configuration of the TCP IP parameters via the front panel is the recommended method for setting up the module s LAN interface On board configuration is only possible during the module s start up procedure 1 Power on the detector and press any front key when the following message is displayed Press a key to enter communication setup If no key is pressed within 5 seconds the ELSD will continue its start up routine The previously stored TCP IP parameters will be used 2 Select LAN using left right arrow keys and press AZ Stop to confirm 3 Select either Static or DHCP automatic IP address assignment and press AZ Stop to confirm 4 If Dynamic IP address is selected the instrument will try to obtain an IP address from the network When successful the detector will continue to the main menu screen 5 If Static IP address is selected the instrument will display the stored static TCP IP settings The detector will use the default TCP IP settings if no IP address has been programmed previously see Table 4 on page 35 6 To enter a new IP address use the up down arrow keys 7 To enter a new Subnet Mask use the up down arrow keys 8 To enter a new Gatew
45. fested by loss of signal increased baseline noise and in the extreme case gas bubbling out of the nebuliser drain tube If this happens proceed as follows 1 Increase the gas flow to 2 8 SLM and increase the evaporator to maximum temperature The diffuser will be dried out and the instrument ready to use after approximately 1 h under these conditions 2 Reset the instrument to the correct operating conditions and allow to stabilize before continuing Agilent 1200 Infinity Series ELSD User Manual 103 9 Maintenance Cleaning Evaporator Tube 104 If the evaporator tube becomes contaminated with non volatile material resulting in poor chromatography it is recommended that the instrument is initially washed with a solvent suitable for the contamination or a 1 1 mixture of acetone water Depending on usage it is recommended to clean the evaporator tube once a week or every 40 h of use as a preventative routine It is also recommended to clean the unit following the use of buffers If cleaning the unit does not cure the problems then consult Agilent Technologies for further assistance Do not use solvents that contain additives when performing the cleaning procedure Ensure that the instrument is at equilibrium under the above conditions before leaving the instrument unattended 1 Set the evaporator temperature to 40 C the nebuliser temperatures at 40 C and the gas flow to 2 8 SLM 2 Pump the cleaning solvent into
46. ge thus the recorded baseline position will remain unchanged Confirmation of a PMT change will be obvious by the change in baseline noise Agilent 1200 Infinity Series ELSD User Manual 57 5 58 Using the Module Response Time Smoothing The data outputted from the detector can be averaged to produce a smoother response The smoothing width is set to the number of data points over which the data is averaged and can be regarded as a digital time constant The smoothing range is settable from 1 50 Gn increments of 1 which translates to 0 1 5 0 s For most HPLC applications the default value of 30 3 s is satisfactory However for faster separations where peak widths lt 3 s a setting of 1 0 1 s is recommended For GPC applications where peak widths can be gt 30 s a value of 50 5 s is recommended Light Source Intensity LED The G4260B ELS detector s LED intensity can be adjusted in order to bring the peak response back on scale The intensity range can be set between 1 100 with the default factory setting being 100 for maximum sensitivity The LED setting is stored in memory and is retained even after a power on off cycle This feature is extremely useful for preparative chromatography where samples of high concentration can be analyzed which would otherwise exceed the dynamic range of the detector The Agilent 1260 Infinity ELSD G4260B performs an automatic auto zero i e 10 mV following an LED cha
47. have a separate written agreement with warranty terms covering the material in this document that conflict with these terms the warranty terms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcon tract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commercial item as defined in FAR 2 101 a or as Restricted computer soft ware as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or dis closure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly per formed or adhered to
48. he ChemStation and EZChrom drivers are only applicable with the following ELSD firmware revisions EZChrom Firmware v30 0 0 or higher e ChemStation with RC Net driver Firmware v30 0 0 or higher 64 Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 General Considerations The ELS Detector should be thought of as a detector like any other designed for liquid chromatography The main distinguishing feature is the ability to evaporate the solvent from the column eluent Therefore normal system set up precautions should be remembered when starting to use the instrument Any solvent intended for use with the ELSD should be fully miscible with any previously used in the liquid chromatograph if there is any uncertainty then a mutually miscible solvent should be run through the system as an intermediate liquid The sample loop should also be flushed with miscible solvent where necessary The intended eluent should be thoroughly degassed contain no non volatile salts or material and should be fully compatible with the column s All connections should be made with zero dead volume fittings and tubing with an I D 0 254 mm S0 010 in The ELSD requires nitrogen of purity gt 98 at an inlet pressure of 4 6 7 bar If in house nitrogen is not available then we recommend the use of a nitrogen generator a constant uninterrupted supply of high purity gas Air can be used with non flammable solvent systems The eluent of choice sh
49. he module logbook 86 Agilent 1200 Infinity Series ELSD User Manual Error Information 8 Module Specific Error Messages These errors are detector specific Internal temperature exceeded lower limit Error ID 10 Air temperature inside the instrument is lt 10 C Probable cause Suggested actions 1 The environmental temperature is outside e Increase ambient temperature where the specified operating limits of the detector is located instrument e Move the detector to a warmer location Internal temperature exceeded upper limit Error ID 11 Air temperature inside the instrument is gt 40 C Probable cause Suggested actions 1 The environmental temperature is outside e Decrease ambient temperature where the specified operating limits of the detector is located instrument Move the detector to a cooler location Agilent 1200 Infinity Series ELSD User Manual 87 88 Error Information On board Vapor sensor failed Error ID 12 The vapor sensor located on the main control board has failed Probable cause Suggested actions 1 Vapor sensor not connected to the main board Please contact your Agilent service representative 2 Defective vapor sensor Please contact your Agilent service representative Rear Vapor sensor failed Error ID 13 The vapor sensor located on the rear panel of the module has failed Probable cause Suggested actions 1 Vapor sensor not connected to the main board Please contact your Agilent se
50. l 30 15 00 hex Option E Binary 10 Select the firmware hex file and click Open The download will begin straightaway and progress will be displayed as shown W Tera Term Send file Filename Main_Control 30 15 00 hex Fullpath C Users Desktop Bytes transfered 1968 17 0 Pause Help e Agilent 1200 Infinity Series ELSD User Manual 109 9 Maintenance Replacing Detector Firmware NOTE Do not disconnect or turn off the detector during the transfer process 11 On successful completion of the file transfer the software will display a Flash memory updated ok message a x r _ COM3 57600baud Tera Term VT E mts PO P ty p File Edit Setup Control Window Resize Help Agilent ELSD Main Bootloader 66 61 62 file transfer updated ok Main Bootloader 66 61 62 Select item 12 Power cycle the module and check that the firmware version displayed on the ELSD front panel at boot up is correct 110 Agilent 1200 Infinity Series ELSD User Manual 7 Agilent 1200 Infinity Series ELSD User Manual KP e ee 10 7 e Parts and Materials for Maintenance amp o e e e Identifying Parts and Materials 112 This chapter provides information on parts for maintenance a Agilent Technologies 111 10 Parts and Materials for Maintenance Identifying Parts and Materials p n Description G4260B Agilent 1260 Infinity Evaporative Light
51. lent 1260 Infinity Evaporative Light Scattering Detector Agilent 1290 Infinity Evaporative Light Scattering Detector Electronic Operation Manual supplied on CD RS232 communication cable LAN shielded cable 1200 Series to ELSD Trigger Cable Gas inlet tube 2 m Rear exhaust hose PVC 2 m Solvent waste tube 1 9 m One power cord region dependant ELSD Software Drivers 27 3 Installing the Module Installing the Module Connecting the Detector to your LC System The ELS detector must be installed by an Agilent service representative Your Agilent service representative will Unpack the ELSD Remove all packing list items that are shipped with the instrument and present them to you for review e Unpack the accessories supplied with the instrument and check that you have received everything on the packing lists Install your ELS detector Place the module on the bench in a vertical position Connect the power cord to the IEC inlet at the rear of the unit Ensure the power switch of the module is OFF switch stands out Connect the power cable to the power connector a A O N Attach the 4 mm OD gas tube into the gas inlet port at the rear of the instrument The gas connection is a push in fitting 6 Connect the solvent waste tube to the waste outlet at the front of the detector and position the other end into a waste collection bottle 7 Connect the front outlet tube to the waste bottle using the supplied tubing
52. m 0 005 in ID tubing placed between the pump and the column Agilent 1200 Infinity Series ELSD User Manual Optimizing Performance 6 Mobile phase priming The ELS detector does not require any mobile phase priming other than that required to prime the solvent through the pump damper injector column etc It is recommended that priming of the LC system be performed without the ELS detector attached to prevent non volatile impurities contaminating the ELS detector The mobile phase should be degassed and filtered either by sparging with Helium or using an on line degasser Agilent 1200 Infinity Series ELSD User Manual 73 Optimizing Performance Solvent recommendations 74 The maximum operating temperature of the detector and the boiling point of the solvent will determine the type of solvents compatible with the ELS detector High boiling point solvents such as e N methylpyrrolidone NMP e Dimethylsulphoxide DMSO meta Cresol m Methylphenol and e 1 2 4 Trichlorobenzene TCB are not recommended Greater care and attention to instrument cleaning procedures should be exercised with these solvents It is recommended that any solvent be flushed from the detector for overnight and weekend storage Agilent 1200 Infinity Series ELSD User Manual Agilent 1200 Infinity Series ELSD User Manual Troubleshooting and Diagnostics Troubleshooting 76 Troubleshooting an HPLC System 77 General Problems 78 Baseline noise 7
53. mage 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 Agilent 1200 Infinity Series ELSD User Manual 19 2 Site Requirements and Specifications CAUTION Inaccessible power plug In case of emergency it must be possible to disconnect the instrument from the power line at any time gt Make sure the power connector of the instrument can be easily reached and unplugged gt Provide sufficient space behind the power socket of the instrument to unplug the cable Power Cords Your detector is delivered with a power cord which matches the wall socket of your particular country or region The plug on the power cord which connects to the rear of the instrument is identical for all types of power cord 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 fun
54. nge in order to keep the signal on scale The Agilent 1290 Infinity ELSD G4261B Laser light source does not have power adjustment Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 Power Mode The instrument can be configured from the front panel sub menu see Sub Menu Screen on page 51 to start in either RUN or STANDBY mode when the unit is switched on via the rear power button To configure the Power Mode select the required Status Mode i e STANDBY or RUN you wish the unit to start up in from the sub menu screen see Sub Menu Screen on page 51 The selected option will take effect the next time the module is powercycled If RUN mode is selected as the desired Power mode then the instrument will use the operating parameters stored in memory In the unlikely event that the instrument encounters a fault during power up the unit will automatically switch to STANDBY mode Data Output Rate Hz The rate at which the ELS Detector outputs data can be selected from the sub menu screen A 10 Hz output rate is selectable for standard LC applications a 40 Hz output rate can be chosen for faster LC separations and 80 Hz is used for UHPLC type applications with very narrow peaks The data rate is stored in memory and is retained even after a power on off cycle The default value is 40 Hz All ELSD conditions are retained on power cycling of the ELSD detector Agilent 1200 Infinity Series ELSD User Manual 59
55. ody When pure solvent is being evaporated only its vapor passes through the light path and the amount of light scattered to the photomultiplier is small and gives a constant baseline response When a non volatile solute is present a particle cloud passes through the light path causing light to be scattered This scattered light enters the optical aperture of the detection system and generates a signal response from the photodiode in real time The quantity of light detected is dependent on the solute concentration and solute particle size distribution 1 Nebulization 2 Evaporation 3 Detection Figure 1 Principles of Operation Agilent 1200 Infinity Series ELSD User Manual Introduction to the Detector 1 Theory There are four main processes by which the path of electromagnetic radiation or light can change direction when passing through a medium containing a suspended particulate phase see Figure 2 on page 11 Reflection Refraction Rayleigh es aie Figure 2 ELSD Scattering Mechanisms The importance of each of these processes depends on the radius of the particle r compared to the wavelength A of the incident light Rayleigh scattering is predominant when r A is lt 5 10 When particle dimensions are greater than A 20 they no longer behave as point sources and Mie scattering becomes predominant Once particle size approaches the wavelength of incident light then reflection and refraction begin to prevail The rel
56. of range or communication failed 93 cooled evaporator temperature problem 84 120 D data output rate 59 defect on arrival 26 delivery checklist 27 detector operation 31 detector sensitivity 12 detector front view 13 overview 13 rearview 14 diffuser drying 103 dimensions 22 display noton 83 display screen 50 drying diffuser 103 E electronic waste 117 electrostatic discharge ESD 100 error conditions 54 error messages communication to laser failed 94 cooled evaporator current out of range or communication failed 93 evaporator gas flow rate limit exceeded 91 evaporator temperature limit exceeded 91 fan failed on cooled evaporator 92 fan failed 89 fan stopped 90 internal temperature exceeded lower limit 87 internal temperature exceeded upper limit 87 invalid evaporator temperature 92 invalid nebulizer temperature 92 laser current out of range 93 laser interlock open or failed 94 laser temperature out of range 93 leak detected 89 leak sensor failed 95 LED light source error 91 nebulizer temperature limit exceeded 90 on board vapor sensor failed 88 rear vapor sensor failed 88 vapor detected 88 error clearing 54 evaporator gas flow rate limit exceeded 91 evaporator temperature limit exceeded 91 evaporator temperature zero 83 evaporator temperature 12 56 evaporator tube cleaning 104 F fan failed on cooled evaporator 92 fan failed 89 fan stopped 90 firmware replacing 106
57. on setup for the 1290 Infinity ELSD detector G4261B using LAN as the communication method 1 Open the Instrument Configuration window LC System G4289C a _ ics mn F L system 42900 gaine fE system 642920 Ei sistem o42548 Generic Modules G4260A G4261A Agilent 1260 Infinity ELSD G4260B Agilent 1290 Infinity ELSD G4261B a I Selected Modules Agilent LC Modules and Systems 4 VWD G1314C DEAAV00101 2 HiP Sampler G1367B DE64455000 6 Quat Pump G1311A DE62972707 Generic Modules P ELSD G4261B noncooled 4 Go c e 2 Select the required ELSD module and choose Configure to set the communication parameters Configurable Modules LC System G4289C 7 E Fic ston 622500 Configuration Fj system 42230 LC System G4294B Generic Modules _ MEE Coe G4260A G4261A Agilent 1260 Infinity ELSD a 642608 Agilent 1290 Infinity ELSD G4261B Selected Modules Agilent LC Modules and Systems Vy VWD G1314C DEAAVO00101 2 HiP Sampler G1367B DE64455000 Quat Pump G1311A DE62972707 Generic Modules l a G 3 Select the instrument Type ID according to the ELSD model connected Agilent 1200 Infinity Series ELSD User Manual 45 4 LAN Configuration PC and Agilent ChemStation Setup 4 Select IP Address and enter the module s IP a
58. ons Increase the evaporator temperature and or gas flow Use a lower concentration of stabiliser unstabilised solvent or a more volatile buffer ammonium acetate or ammonium formate Perform cleaning procedure Refer to local distributor or Agilent Technologies Suggested actions Increase evap gas flow rate Optimize HPLC separation Suggested actions Stop pump flow and switch off unit Restart unit and A Z without liquid flowing e Refer to local distributor or Agilent Technologies Optical section contaminated and requires cleaning 81 7 Troubleshooting and Diagnostics No power Probable cause 1 Mains lead not connected 2 Fuse failure 3 Power supply failure Suggested actions Attach mains lead to socket and inlet on rear of instrument Replace fuse Call Agilent Service representative No response completely flat baseline Probable cause 1 Data acquisition leads not connected 2 Light source inactive 3 Output below 0 mV 4 Instrument in STANDBY mode 82 Suggested actions Ensure connectors to computer or integrator are sound e Check LED intensity is 100 Check LED or LASER is functioning correctly by stopping solvent flow cycling the power Then reading the offset value in RUN mode Stop pump flow and A Z without liquid flowing Select RUN mode Agilent 1200 Infinity Series ELSD User Manual Troubleshooting and Diagnostics 7 Temperature error as soon as instrument
59. ontains additional firmware on the peltier unit and the Laser assembly Firmware on all three assemblies can be upgraded using the same process Firmware upgrade is only possible via the serial port For majority of internal repairs Description Allen keys TERA TERM software Current firmware file Description Serial cable supplied with instrument Firmware versions v24 0 4 for the 380 ELSD and v24 0 2 for the 385 ELSD or later are not compatible with 1260 and 1290 Infinity models To upgrade downgrade the modules firmware carry out the following steps 1 Connect the detector to a PC via the serial port on the rear of the module using a RS232 cable 2 Open the Tera Term program and select File gt New Connection from the toolbar Agilent 1200 Infinity Series ELSD User Manual Maintenance 9 3 Select Serial and choose the appropriate COM port followed by OK Tera Term New connection z TCP IP Ho 192 168 1 3 History Telnet oraa gt SSH 3SH version SSH2 Other rotocol UNSPEC Serial Port COM1 Communications Port COM1 Cancel Help 4 From the toolbar menu select Setup gt Serial Port to configure the serial port connection 5 Set the Serial port to the parameters shown below and click OK Tera Term Serial port setup z Port COM1 X a Baud rate 57600 X Data 8 bit X Cancel Parity none v Stop Ibit Help Flow cont
60. ould be fully volatile under the chosen detector parameters any non volatilized eluent will increase baseline noise and reduce sensitivity The ELS Detector is a destructive technique and must be placed last when used in series with other detectors Agilent 1200 Infinity Series ELSD User Manual 65 5 66 Using the Module Solvent Recommendations Any solvent intended for use with the ELS Detector should be thoroughly degassed filtered 0 45 um and fully compatible with the column s Solvents that are not properly degassed may cause problems at nebulization leading to a poor reproducibility Non Volatile buffers are not compatible with the ELS Detector and should not be used Only volatile mobile phase additives such as those listed in Table 6 on page 67 should be used with the ELS detector Tetrahydrofuran THF stabilized with BHT may increase the baseline noise level Where possible unstabilized THF should be used with the ELS detector High boiling point solvents such as N methylpyrrolidone NMP Dimethylsulphoxide DMSO m Cresol and 1 2 4 Trichlorobenzene TCB are not recommended Greater care and attention to instrument cleaning procedures should be exercised with these solvents Sample Preparation Samples containing particulate matter should be filtered through a 0 45 um filter prior to injection Column Considerations The ELS detector will detect all non volatile components in the mobile phase which incl
61. rformance Liquid Chromatography HPLC The solvent stream containing the solute material is nebulized and carried by a gas flow through an evaporation chamber The solvent is volatilized leaving a mist of solute particles that scatter light to a photosensitive device The signal is amplified and a voltage output provides the concentration of the solute particles passing through the light The Agilent 1260 1290 Infinity ELSD may be used alone or as one of several detectors in a GPC or HPLC system As the solvent or eluent is evaporated in the course of the analysis the Agilent 1260 1290 Infinity ELSD must be the last in series if used in conjunction with other detectors If the Agilent 1260 1290 Infinity ELSD is being used as the last detector in a series care must be taken not to exceed the recommended backpressure in detector cells in other units This manual instructs the user in the installation and operation of the Agilent 1260 1290 Infinity ELSD for stand alone use and control using Agilent OpenLAB ChemStation and EZChrom editions and Agilent ChemStation Agilent 1200 Infinity Series ELSD User Manual Introduction to the Detector 1 System Overview Basic Principles of Operation Nebulization The eluent inlet is connected to the nebuliser via a short length of stainless steel capillary tube The incoming eluent stream passes through the heated nebuliser and is mixed with the incoming nebuliser gas stream The mixed gas and eluen
62. rigger cable PL0890 0345 Agilent 1200 Infinity Series ELSD User Manual 61 5 62 Using the Module Creating a Real time Program In order to create or modify the on board timetable DIMENSION software must be installed on your PC The DIMENSION software package allows you to create a timetable on a PC which can subsequently be downloaded to the ELSD for later use The DIMENSION software also allows you to delete a time table from the ELSD detector memory The ELSD can only store a single timetable in memory so the DIMENSION software can be used to create and save multiple timetables that can be downloaded individually at a later date For further information on how to use DIMENSION software please refer to the DIMENSION software on line help Dimension software can only communicate with the ELSD using the Serial port LAN communication is not supported in DIMENSION Starting and Stopping Real time Control The ELSD contains an internal timer to initiate the time based events stored within the timetable To start the internal timer and trigger the on board timetable a contact closure input via the I O connector on the rear of the instrument is required see Overview of ELS Detector on page 13 When the on board timetable is triggered the front panel of the ELSD will display TTRUN above the output as shown in Figure 11 on page 63 When the timetable is running the current and the total run time are displayed
63. rol none Transmit delay 1 msecjchar 20 msecjline Transmit delay should be set to 0 msec char when downloading Main control Firmware 6 Put the detector into Service mode by holding down the rear Flash button whilst switching on the module The front panel will display SERVICE MODE Reboot for normal operation Agilent 1200 Infinity Series ELSD User Manual 107 9 Maintenance Replacing Detector Firmware When in Service mode the Tera Term displays the bootloader version and firmware menu W COM3 57600baud Tera Term VT File Edit Setup Control Window Resize Help igilent ELSD Main Bootloader 66 01 82 Ly Main Safety Laser Select item 7 Select the firmware you wish to upgrade downgrade by pressing the appropriate number e g press 1 to upgrade the main control firmware 8 Press U to begin the update process Select item m r Main Bootloader 88 01 02 Application 6 1 8 Press lt U gt to update or lt B gt to go back to menu Awaiting hex file transfer 108 Agilent 1200 Infinity Series ELSD User Manual Maintenance 9 Replacing Detector Firmware 9 To choose the firmware file select the Send File option from the File menu in the toolbar and navigate to the folder where the file is located l Tera Term Send file Look in Jo Main Fd e flv Name Date modified _ Main_Control 30 15 00 hex 08 08 2012 09 18 4 w File name Main_Contro
64. rs as a malfunction of the ELS Detector To troubleshoot the ELS Detector you must be able to separate the performance of the ELS Detector within the HPLC system from its performance outside the HPLC system This section begins with guidelines for testing the ELS Detector as a stand alone See Module Specific Error Messages on page 87 for possible cause and suggested solution Agilent 1200 Infinity Series ELSD User Manual Troubleshooting and Diagnostics 7 Troubleshooting an HPLC System Standard practice is to add one component at a time back into the HPLC system so that the component causing the problem is easily identified if when the condition reoccurs Begin troubleshooting by adding the pump to the ELS Detector first and finish by adding the column last If another type of detector is available use it before the ELS Detector to aid in troubleshooting Agilent 1200 Infinity Series ELSD User Manual 77 7 Troubleshooting and Diagnostics General Problems Baseline noise Probable cause 1 Poor nebulisation 2 Insufficient evaporation 3 Non volatile additive in mobile phase 4 Pressure difference created inside nebuliser chamber 5 Pump pulsations especially in microbore applications where low flow rates are used 78 Suggested actions Increase the temperature of the nebulizer by 10 C until the baseline noise decreases Increase the temperature of the evaporator by 10 C until the baseline noise decrea
65. rvice representative 2 Defective vapor sensor Please contact your Agilent service representative Vapor detected Error ID 14 Solvent vapor threshold exceeded inside module Probable cause Suggested actions 1 External vapor being drawn into unit Remove any source of solvent vapours close to the module 2 Solvent leak inside unit Please contact your Agilent service representative 3 Exhaust tube not fitted Fit black exhaust tube Agilent 1200 Infinity Series ELSD User Manual Error Information 8 Leak detected Error ID 15 A leak was detected inside the module Probable cause Suggested actions 1 Loose nebuliser fittings Please contact your Agilent service representative 2 Blocked nebuliser causing leak at capillary Please contact your Agilent service fittings representative Fan Failed Error ID 16 Thermal shut down of the main cooling fan Probable cause Suggested actions 1 Fan cable disconnected Please contact your Agilent service representative 2 Defective fan Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative Agilent 1200 Infinity Series ELSD User Manual 89 8 Error Information Fan Stopped Error ID 17 A main cooling fan in the module has stopped Probable cause Suggested actions 1 Obstruction of fan blades Please contact your Agilent service representative 2 Defective fan Please contact your Agilent service repr
66. s ELS detectors or other designs of ELSD e g Agilent G4218A ELSD to the ELSD will not provide equivalent performance As stated in Basic Principles of Operation on page 9 the operating temperatures of the ELS detector are set according to the type of analyte and not the mobile phase composition as with other ELS detectors For example when HPLC grade water is used as the mobile phase the Agilent G4218A ELSD requires an evaporation temperature between 35 40 C Whereas the Agilent G4261B can be operated as low as 20 30 C for the equivalent solvent Therefore the transfer of operating conditions from other models of ELSD to the ELSD is not valid and the only way to ensure that the detector will provide the optimum analyte signal to noise is to follow the guidelines outlined in Operational Parameters on page 12 Agilent 1200 Infinity Series ELSD User Manual Agilent 1200 Infinity Series ELSD User Manual 6 Optimizing Performance Do s and Don ts of ELS Detection 70 Location of the Detector Module 71 Pumping systems 72 Mobile phase priming 73 Solvent recommendations 74 This chapter gives hints on how to optimize the performance or use additional devices ott Agilent Technologies 69 6 Optimizing Performance Do s and Don ts of ELS Detection CAUTION Decreased performance High pressures on the internal chamber will lead to increased baseline noise and low sensitivity gt NEVER block the exhaust
67. sembly not connected to main Please contact your Agilent service board representative 3 Defective main board Please contact your Agilent service representative Laser temperature out of range Error ID 26 Temperature control on Laser assembly outside of normal operating range Probable cause Suggested actions 1 Defective Laser assembly Please contact your Agilent service representative Laser current out of range Error ID 27 Laser current outside of normal operating range Probable cause Suggested actions 1 Defective Laser assembly Please contact your Agilent service representative Agilent 1200 Infinity Series ELSD User Manual 93 94 Error Information Laser interlock open or failed Error ID 28 The laser interlock on the detector enclosure is open or failed Probable cause Suggested actions 1 Module enclosure is open Please contact your Agilent service representative 2 Interlock not connected to main board Please contact your Agilent service representative 3 Interlock wiring is faulty Please contact your Agilent service representative 4 Defective main board Please contact your Agilent service representative Communication to Laser failed Error ID 29 Communication between main board and laser assembly has failed Probable cause Suggested actions 1 Laser assembly not connected to main Please contact your Agilent service board representative 2 Defective Laser assembly Please contact your Agilent
68. ses e Increase the evaporation gas flow rate Decrease the nebulisation temperature Use a volatile mobile phase as shown Ensure that the end of the liquid waste tube is not immersed in liquid Ensure that the exhaust tube at rear of unit is not blocked or extraction is too strong e Use a pulse free pump Increase the back pressure on the pump by fitting a back pressure column between the pump and the injection valve Use a pulse dampener directly after the pump in the system Agilent 1200 Infinity Series ELSD User Manual Baseline spikes Probable cause 1 Particulate matter in the gas supply 2 Column shedding 3 Poor nebulisation 4 Insufficient evaporation 5 Non volatile additive in mobile phase Troubleshooting and Diagnostics 7 Suggested actions Filter the incoming gas or change the supply Replace column or fit an inline filter with a 0 2 um membrane filter directly after the column Check solvent flow rate into ELSD is constant Check inlet gas flow is gt 60 psi and stable Increase the temperature of the evaporator by 10 C until the baseline noise decreases Replace additive in mobile phase with volatile buffer Low sensitivity and baseline noise drift Probable cause 1 Diffuser saturated with solvent Agilent 1200 Infinity Series ELSD User Manual Suggested actions Stop the eluent flow and increase the evaporator temperature to maximum Increase the flow rate to 2 8 SLM and w
69. sistors to 5 V For ELS Detector 1 0 connections see Table 1 on page 15 13 Install ELSD drivers for full control via OpenLab CS or EZChrome 14 Connect the LC column outlet to the eluent inlet at the front of the unit using the shortest length of tubing possible 1 16 in OD 0 010 in ID The eluent from the chromatography system is connected to the central front port of the ELS Detector via a low dead volume Valco bulkhead connector The liquid inlet port is connected directly to the nebuliser by a short length 130 mm of capillary tube giving a delay volume from port to nebuliser tip of 4 pL 15 Turn on the source gas to a pressure of about 4 1 6 9 bar Agilent 1200 Infinity Series ELSD User Manual Installing the Module 3 Checking Operation of the ELS Detector 1 Switch on the ELS Detector If using OpenLAB CDS ChemStation or EZChrom the front panel keypad will become locked when launching the software 2 In ChemStation or EZChrom set operational parameters i e nebuliser and evaporator temperature and download them to the instrument Then turn the ELS detector status to On For control outside of ChemStation and EZChrom use the front panel to change the ELS detector settings Initiate heating by selecting RUN mode using the arrow keys on the front keypad When the unit has reached temperature the baseline noise should be checked to ensure that it is lt 0 2 mV peak peak This verifies that the gas supply is
70. t stream form an aerosol plume containing a uniform dispersion of droplets that then passes as a continuous flow into the evaporator section Any larger droplets or the inefficiently nebulized droplets collect in the nebuliser chamber waste trap and then drain off via the waste outlet into a collection bottle Evaporation After nebulization the atomized spray is propelled through the evaporation tube assisted by the carrier gas In the evaporator section the solvent is removed leaving a stream of dry particles of the analyte A diffuser located in the evaporator assists in the drying of the particles acting as an efficient heat exchanger prevents ballistic particles reaching the scattering chamber and randomizes the particle plume The ELS Detectors use patented gas flow technology in the evaporation zone to aid evaporation at low temperatures By adding a stream of dry nitrogen evaporation gas at the entrance of the evaporator tube less volatile solvents for example water are easily evaporated This evaporation gas is controlled by the user and facilitates sub ambient operation Agilent 1200 Infinity Series ELSD User Manual 9 1 10 Introduction to the Detector Detection Light in the optical chamber is passed through the instrument at right angles to the direction of particle flow A light trap is located opposite the source of light to capture the transmitted incident beam eliminating internal reflections within the instrument b
71. the changes 7 Select Logout to close the session 8 Restart the module for the new TCP IP settings to be implemented 38 Agilent 1200 Infinity Series ELSD User Manual LAN Configuration 4 Contact your system administrator for assistance on configuring the detector s network settings Changes to the TCP IP parameters other than those described could render the ELSD inoperable With Telnet Whenever a TCP IP connection to the module is possible TCP IP parameters set by any method the parameters may be altered by opening a Telnet session 1 Open the system DOS prompt window by clicking on Windows Start button and select Run OR Press the Windows button and R simultaneously and click OK 2 Type the following into the RUN dialog Telnet lt IP Address gt Telnet lt host name gt Run Sa m Type the name of a program folder document or Internet resource and Windows will open it for you Open elnet 156 141 59 43 X Figure 5 Starting a Telnet session where lt IP address gt may be the assigned address via the instrument a configuration session using the web interface of the default IP address see Table 4 on page 35 If Telnet is not installed on your PC by default you can turn on the feature via Windows Control Panel Agilent 1200 Infinity Series ELSD User Manual 39 4 LAN Configuration When the connection is established successfully the module responds with the following
72. the instrument at 1 2 mL min whilst in the RUN mode overnight or for a minimum of 4 h if overnight operation is not possible Agilent 1200 Infinity Series ELSD User Manual Maintenance 9 Putting the Instrument into Storage If the instrument is to be stored or not used for an extended period of time it is recommended to follow the procedure outlined below 1 Flush the detector with a mixture of Acetone Water 50 50 at 1 mL min for 15 min Allow the instrument to cool to ambient temperature in STANDBY mode with the gas supply still connected Tip the instrument forwards to try and empty the solvent within the nebulization chamber through the front waste tube i e into the bottle Pour 10 20 mL of acetone into the rear exhaust tube to flush out the internal solvent trap collecting any overflow of acetone at the front solvent pipe Repeat step 3 to drain the acetone 6 Disconnect the waste bottle Using the gas supply blow nitrogen gas through the exhaust to evaporate any remaining acetone in the solvent trap Cover the waste tube with tissue paper to collect any acetone residue Plug the exhaust waste tubes and solvent inlet with the plastic caps provided Agilent 1200 Infinity Series ELSD User Manual 105 9 Maintenance Replacing Detector Firmware When Tools required Parts required 106 The ELSD contains control firmware that can be flash upgraded The Agilent 1290 Infinity ELSD G4261B also c
73. tifying 112 missing 27 peak tailing 81 physical specifications 22 PMT 57 power consideration 19 power consumption 22 power cords 20 power mode 59 power switch 28 pre installation requirements 18 preparation sample 66 priming 73 principle of operation 9 pump 72 real time control starting 62 stopping 62 real time program creating 62 rear vapor sensor failed 88 replacing firmware 106 requirements pre installation 18 response time 58 121 Index S safety class 115 safety general information 115 standards 22 symbols 114 site requirements 17 power cords 20 smoothing 58 solvent recommendation 66 74 specification physical 22 specifications 17 performance 23 spiky peak tops 80 status mode 53 storage 105 sub menu screen 51 T TCP IP parameter configuration using front panel 36 using web browser 37 with telnet 39 TCP IP settings 60 local configuration 42 temperature error 83 temperature methods transfer 68 temperature 56 troubleshooting error messages 86 HPLC system 77 U unpacking 26 122 V vapor detected 88 vapor sensor error 84 voltage range 22 wW waste electrical and electronic equipment 117 WEEE directive 117 weight 22 Agilent 1200 Infinity Series ELSD User Manual Index Agilent 1200 Infinity Series ELSD User Manual 123 www agilent com In This Book This manual contains information on the Agilent 1260 Infinity Evaporative Light Scattering Detector G4260B and
74. tions 2 The instrument is suitable for indoor use only and is classified suitable under the following categories EN 61010 1 2010 e Installation category II e Pollution degree 2 Safety class 1 Table3 Performance Specification of the ELS Detector Type Specification Light Source G4260B LED 480 nm Class 1 LED product G4261B LASER 405 nm 10 mW Class 3B Detector PMT with digital signal processing Nebuliser OFF 25 90 C Evaporator Non cooled OFF 25 120 C Cooled OFF 10 80 C Gas Flow Range Operating Pressure Eluent Flow range Digital Output Analogue Output Communication 0 9 3 25 SLM controlled gas shut off 60 100 psi 4 6 7 bar 0 2 5 0 mL min 10 40 or 80 Hz 24 bit 0 1 25 V FSD Ethernet Serial RS232 Remote Start Input Pump Stop 1 Contact closure Agilent 1200 Infinity Series ELSD User Manual 23 2 24 Site Requirements and Specifications Table3 Performance Specification of the ELS Detector Type Specification PC control software Remote operation Safety features ELSD driver for Rev B ChemStation RC NET driver ELSD driver for OpenLAB ChemStation edition ELSD driver for OpenLAB EZChrom edition ELSD Dimension Software Remote Start Input Gas shut off Valve Leak Detection Laser Interlock Agilent 1200 Infinity Series ELSD User Manual Agilent 1200 Infinity Series ELSD User Manual e Installing the Module J Unp
75. trumentation product Do not dispose off in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com for more information Agilent 1200 Infinity Series ELSD User Manual 117 11 Appendix Radio Interference Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with equipment unscreened cables and or used for measurements on open set ups the user has to assure that under operating conditions the radio interference limits are still met within the premises 118 Agilent 1200 Infinity Series ELSD User Manual Appendix 11 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 Agilent 1200 Infinity Series ELSD User Manual 119 Index Index A Agilent oninternet 119 ambient non operating temperature 22 ambient operating temperature 22 baseline drift 79 78 79 baseline spikes 79 baseline noise C ChemStation setup 45 cleaning evaporator tube 104 column consideration 66 communication to laser failed 94 communication LAN 49 serial 49 connecting detector to system 28 considerations 65 controlling during injection 61 controlling ChemStation 64 EZChrom 64 cooled evaporator current out
76. udes column packing material Column packing material will become chemically and mechanically broken down over the lifetime of the column causing particles to enter the ELSD This column shedding will lead to extremely high baseline Amino columns used with aqueous mobile phase are particularly prone to this type of shedding and should be checked regularly To minimize column breakdown always follow the manufacturers instruction supplied with the column Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 Table 6 Volatile mobile additives compatible with ELS detection Mobile Phase Additive pKa pKb pH Range Bp C Mp C Acids Trifluoroacetic Acid TFA 0 3 13 70 72 4 15 4 Formic Acid 3 75 10 25 100 7 8 3 Acetic Acid 4 75 9 25 116 0 16 6 Bases Ammonia 9 25 4 75 33 4 71 1 Methylamine 10 66 3 34 6 6 94 0 Ethylamine 10 81 3 19 16 6 81 0 Triethylamine 11 01 2 99 89 3 114 7 Buffers Ammonium Formate 3 8 3 0 5 0 120 9 2 8 2 10 2 Ammonium Acetate 4 8 3 8 5 8 111 9 2 8 2 10 2 Ammonium Bicarbonate 6 3 6 8 11 3 106 9 2 10 3 lon Pair Reagent Pentafluoropropionic acid PFPA 0 6 97 Heptafluorobutyric acid HFBA 0 6 120 Nonafluoropropionic acid NFPA 0 6 140 Tridecafluoroheptanoic acid 0 6 175 Agilent 1200 Infinity Series ELSD User Manual 67 5 68 Using the Module Transferring ELSD Temperature Methods The direct transfer of ELSD operating conditions from other manufacturer
77. ult value is 30 C Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 Evaporator Gas Flow The evaporator gas flow is used to control the ELS detector s evaporation process The evaporator gas value is set according to the mobile phase composition with higher gas flows e g 1 6 SLM being used for aqueous eluent compared to those containing organic solvents The higher the evaporator temperature the lower the evaporation gas setting required e g 1 0 0 9 SLM regardless of mobile phase composition Likewise as the evaporator temperature is reduced to ambient and sub ambient temperatures the gas flow needs to be increased to compensate e g 1 6 1 8 SLM The evaporation gas range for both models is 0 9 3 25 SLM 0 05 increments The default value is 1 6 SLM Detector Gain PMT This parameter sets the factor by which the detector output signal is amplified The gain setting does not change the sensitivity of the detector but merely amplifies the captured signal by the inputted factor The gain can be adjusted from 1 to 10 in increments of 0 1 When setting the PMT or Gain both the signal and noise are simply amplified by the value set so S N values are unaffected The raw signal output displayed on the parameter screen will reflect this increase or decrease in signal amplification Please note that the instrument output displayed on the main operating screen does not alter following a PMT chan
78. wn in Figure 7 on page 50 or via PC control using software e g ChemStation Display Screen Keypad The graphical interface on the front of the instrument displays the current method status evaporator temperature nebuliser temperature gas flow and output of the instrument Operating parameters can be altered via the interactive menu bar at the bottom of the display Figure 7 ELSD Display Screen The four arrows on the front of the instrument are used to navigate within the interactive menu bar The AZ Stop key has a dual function it can be used to auto zero the ELSD at any time unless a timetable is running If the AZ Stop key is pressed during an active timetable the timetable will stop running and the ELSD will revert to STANDBY mode Agilent 1200 Infinity Series ELSD User Manual Using the Module 5 Main menu bar To change the current settings use the arrow keys to navigate across the interactive menu bar until the desired option is flashing Using the up down arrow keys alter the parameter to the desired setting In order to action any changes the cursor must be returned to the Home position or When the cursor is located in the Home position the actual detector values are displayed in the main screen If the instrument is controlled via PC software then the home key will display a locked icon and the keypad will be disabled To unlock the keypad software control must be terminated Sub M

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