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4

Using  the  Module

Instrument Controls

Agilent InfinityLab ELSD User Manual

46

Status Mode

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 corner of the screen.

Standby

The 

STANDBY

 mode is the “ground state” of the ELS detector, which is by default 

selected automatically after power-on (default can be changed using Power 
Mode, 

“Power Mode”

on page 50). 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 parameters (gas flow, nebulizer, and evaporator temperatures) 
before switching the unit into 

RUN

 mode. The instrument will default to 

STANDBY

 

mode should an error occur on the instrument.

Following a command or error, the instrument is switched from 

RUN

 to 

STANDBY

 

mode. In this situation, 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 

STANDBY

 enough to nebulize and 

evacuate solvent should the instrument default to 

STANDBY

 mode with solvent 

still flowing.

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 that the system has not reached the set conditions. When the instrument 
has equilibrated, 

READY

 will be displayed and the instrument is ready for use.

CAUTION

Flooding the detector
If the instrument is left in STANDBY mode for longer than 15 min, gas flow to 
the unit is stopped to minimize gas usage.

The solvent pump must be turned off if the ELSD is going to be left in 
STANDBY mode longer than 15 min to prevent solvent flooding the detector.

Содержание InfinityLab 1290 Infinity II

Страница 1: ...Agilent InfinityLab Evaporative Light Scattering Detectors User Manual Agilent InfinityLab ELSD User Manual ...

Страница 2: ...parate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used orcopied only in accordance with the terms of such license Restricted Rights Legend U S Government Restricted Rights Soft ware and technical data rights granted to the federal government include only those rights customarily provided to end user c...

Страница 3: ...rmance specifications 3 LAN Configuration This chapter provides information on connecting the module to the control software 4 Using the Module This chapter explains the operational parameters of the ELSD 5 Optimizing Performance This chapter gives hints on how to optimize the performance or use additional devices 6 Troubleshooting and Diagnostics This chapter gives an overview about the troublesh...

Страница 4: ...8 Maintenance This chapter describes the maintenance of the ELSD 9 Parts and Materials for Maintenance This chapter provides information on parts for maintenance 10 Appendix This chapter provides addition information on safety legal and Web ...

Страница 5: ...to Do First 28 TCP IP Parameter Configuration 29 PC and OpenLab CDS OpenLab ChemStation or OpenLab EZChrom Software Setup 36 4 Using the Module 41 Before Using the Detector 42 Instrument Controls 43 Operational Parameters 48 Controlling the ELSD During an Injection 52 Controlling the ELSD within OpenLab CDS OpenLab ChemStation or OpenLab EZChrom 54 General Considerations 55 5 Optimizing Performanc...

Страница 6: ...tenance 84 Cautions and Warnings 85 Cleaning the Module 87 Inspection of Cables 88 Drying the Diffuser 89 Cleaning the Nebulizer 90 Cleaning Evaporator Tube 91 Putting the Instrument into Storage 92 Updating Detector Firmware 93 9 Parts and Materials for Maintenance 98 Identifying Parts and Materials 99 10 Appendix 100 General Safety Information 101 Waste Electrical and Electronic Equipment WEEE D...

Страница 7: ...duction to the Detector Introduction to the ELSD 8 System Overview 9 Basic Principles of Operation 9 Operational Parameters 12 Overview of ELS Detector 13 This chapter gives an introduction to the module instrument overview and internal connectors ...

Страница 8: ...vides the concentration of the solute particles passing through the light The Agilent 1260 Infinity II ELSD or Agilent 1290 Infinity II ELSD may be used alone or as one of several detectors in a GPC or HPLC system As the solvent or eluent is evaporated during the analysis the Agilent 1260 Infinity II ELSD or Agilent 1290 Infinity II ELSD must be the last in series if used with other detectors If t...

Страница 9: ...en 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 ...

Страница 10: ...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 nonvolatile 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 ...

Страница 11: ...e 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 relative 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 sourc...

Страница 12: ...ents 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 µm droplet of water at 30 C can be dried ca 3x faster than just temperature alone Using the Agilent 1290 Infinity II ELSD G7102A water can be evaporated as low as 20 C providing maximum sensitivity to therm...

Страница 13: ...InfinityLab ELSD User Manual 13 1 Introduction to the Detector System Overview Overview of ELS Detector Figure 3 ELSD overview front 1 2 3 4 1 Front screen display 2 Keypad 3 Eluent inlet 4 Solvent waste outlet ...

Страница 14: ...tyLab ELSD User Manual 14 Figure 4 ELSD overview rear 1 2 3 4 5 6 7 8 9 1 Vapor Sensor vent 2 Serial RS232 port 3 LAN connector only active on G7102A 4 Firmware button 5 I O connector Remote Start input 6 Mains Switch 7 Mains Input 8 Gas Inlet port 9 Exhaust port ...

Страница 15: ...s Timetable Start 14 ground Injection Sync 13 ground Remote A Z 7 ground Output Pump stop contact closure normally open 3 10 Ground to case 1 5 6 11 NOTE To make appropriate remote start and A Z connections from a third party LC a third party remote start cable for Dimension software Remote start cable PL0890 0350 can be purchased from Agilent Technologies ...

Страница 16: ...fications 21 Physical Specifications Agilent 1260 Infinity II ELSD G4260B 21 Physical Specifications Agilent 1290 Infinity II ELSD G7102A 22 Performance Specifications 23 Performance Specifications G4260B 23 Performance Specifications G7102A 25 This chapter provides information on environmental requirements physical and performance specifications ...

Страница 17: ...Pre installation Requirements Pre installation Requirements For a detailed description of the environmental and operating requirements of the ELSD see the Site Preparation Checklist This manual will give you an overview of the ELS detector and describe its operation in more detail ...

Страница 18: ...t on the IEC inlet fuse holder on rear of unit WARNING Eye damage by laser light Hazardous laser light can injure eyes Do not remove covers and interlocks Observe and note the laser warning signs carefully WARNING Hazard of electrical shock or damage of your instrumentation can result if the devices are connected to a line voltage higher than specified Connect your instrument to the specified line...

Страница 19: ... the Agilent Technologies power cord designed for your region WARNING Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations WARNING Unintended use of power cords Usi...

Страница 20: ...roximately 15 cm 5 9 inches in the rear for air circulation and electric connections If the bench shall carry a complete HPLC system make sure that the bench is designed to bear the weight of all modules The module should be operated in a horizontal position NOTE Agilent recommends that you install the HPLC instrument in the InfinityLab Flex Bench rack This option helps to save bench space as all ...

Страница 21: ...imensions height width depth 420 x 200 x 450 mm 16 5 x 7 9 x 17 7 inches Line voltage 100 120 220 240 V 10 Line frequency 50 or 60 Hz 5 Power consumption 150 W 2A max Ambient operating temperature 10 35 C 50 95 F Ambient non operating temperature 40 70 C 40 158 F Humidity 10 80 r h Non condensing Operating altitude Up to 2000 m 6562 ft Safety standards IEC EN CSA UL Overvoltage category II Polluti...

Страница 22: ...ons height width depth 420 x 200 x 450 mm 16 5 x 7 9 x 17 7 inches Line voltage 100 120 220 240 V 10 Line frequency 50 or 60 Hz 5 Power consumption 150 W 2A max Ambient operating temperature 10 35 C 50 95 F Ambient non operating temperature 40 70 C 40 158 F Humidity 10 80 r h at 35 C 95 F Non condensing Operating altitude Up to 2000 m 6562 ft Safety standards IEC EN CSA UL Overvoltage category II ...

Страница 23: ...izer OFF 25 90 C Evaporator Non cooled OFF 25 120 C Cooled Not Applicable Gas Flow Range 0 9 3 25 SLM controlled gas shut off Short Term Noise 0 2 mV See conditions in Specification Conditions on page 24 Drift 1 mV h See conditions in Specification Conditions on page 24 Operating Pressure 4 1 6 9 bar 60 100 psi Eluent Flow range 0 2 5 0 mL min Digital Output 10 40 or 80 Hz 24 bit Analogue Output 0...

Страница 24: ... frequency and the amplitude of the temperature changes to below 1 C h 1 8 F h Turbulences around one minute or less can be ignored ASTM measurements require that the detector should be turned on enough time before start of testing PC control ELSD driver for OpenLab ChemStation edition ELSD driver for OpenLab EZChrom edition LC and CE Drivers Rev A 02 11 or above Safety and maintenance Gas shut of...

Страница 25: ... 4 orders of magnitude Short Term Noise 0 1 LSU h See conditions in Table 7 on page 26 Drift 1 LSU h See conditions in Table 7 on page 26 Operating Pressure 4 1 6 9 bar 60 100 psi Eluent Flow Range 0 2 5 0 mL min Digital Output 10 40 or 80 Hz 24 bit Remote Operation Remote Start Input Communication Ethernet Serial RS232 Remote Start Input Pump Stop 1 Contact closure PC Control ELSD driver for Open...

Страница 26: ...ions Larger ambient temperature changes will result in larger drift Better drift performance depends on better control of the temperature fluctuations To realize the highest performance minimize the frequency and the amplitude of the temperature changes to below 1 C h 1 8 F h Turbulences around one minute or less can be ignored ASTM measurements require that the detector should be turned on enough...

Страница 27: ...29 Configuration Using Instrument Front Panel 30 Configuration Using Web Browser 31 With Telnet 33 PC and OpenLab CDS OpenLab ChemStation or OpenLab EZChrom Software Setup 36 PC Setup for Local Configuration 36 Agilent ChemStation Setup 38 This chapter provides information on connecting the module to the control software ...

Страница 28: ...ther 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 30 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 ...

Страница 29: ...ameters through the G7102A ELSD web interface 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 8 on page 29 When configured to obtain its IP address automatically the module will request an IP address from the DHCP server after every power cycle NOTE If the dete...

Страница 30: ...tic IP address is selected the instrument will display the stored static TCP IP settings 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 Gateway address use the up down arrow keys 9 When all values are populated press AZ Stop to accept The instrument will continue to the main menu screen to confirm that the settings ha...

Страница 31: ...b 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 If communication is successful the following login screen will appear 2 To log in type the following information Username user Password Agilent NOTE The default host name is configured to the detector s serial number NOTE The login details a...

Страница 32: ... 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 6 Select Apply again to confirm the changes 7 Select Logout to close the session 8 Restart the module for the new TCP IP settings to be implemented NOTE Contact your system administrator for assistance on configuring the detector s network settin...

Страница 33: ... R simultaneously and click OK 2 Type the following into the RUN dialog box Telnet IP Address Telnet host name _ this can be set manually Figure 5 Starting a Telnet session Where IP address may be the assigned address via the instrument a configuration session using the Web interface of the default IP address see Table 8 on page 29 When the connection is established successfully the module respond...

Страница 34: ...Value Description set network displays syntax and descriptions of commands set network displays the current settings and list of commands set network ip x x x x sets new ip address set network submask x x x x sets new subnetmask set network gateway x x x x 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 fr...

Страница 35: ...etwork ip 156 141 59 43 Then press Enter Parameter refers to the configuration parameters that 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 Enter to exit 7 Restart the module for the new TCP IP settings to be implemented ...

Страница 36: ...tation or OpenLab EZChrom Software Setup 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 8 on page 29 1 Open the Local Area Connection Properties and select Internet Protocol TCP IP Then select Properties ...

Страница 37: ...or OpenLab EZChrom Software Setup 2 Select Alternative Configuration 3 Enter the following IP and subnet mask address for the PC IP address 192 168 254 1 Subnet mask 255 255 255 0 4 Click OK to save the configuration NOTE It can take several seconds for the alternative network settings to take effect ...

Страница 38: ...ure describes the Agilent OpenLab ChemStation setup for the 1290 Infinity II ELSD detector G7102A and 1260 Infinity II ELSD G4260B using LAN as the communication method 1 Open the Instrument Configuration window 2 Select the required ELSD module and click Configure to set the communication parameters 3 Select the instrument Type ID according to the ELSD model connected ...

Страница 39: ...SD User Manual 39 3 LAN Configuration PC and OpenLab CDS OpenLab ChemStation or OpenLab EZChrom Software Setup 4 Select IP Address and enter the module s IP address OR Select Hostname and enter the instrument s serial number ...

Страница 40: ... model option if required 6 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 communication with the software might be prevented following a power cycle of the instrument Recommend using a static IP address to ensure communication with the software is preserved after power cycle ...

Страница 41: ...in PMT 49 Response Time Smoothing 50 Light Source Intensity LED 50 Power Mode 50 Data Output Rate Hz 51 LAN TCP IP Settings 51 Controlling the ELSD During an Injection 52 Real Time Operation 52 Creating a Real Time Program 52 Starting and Stopping Real Time Control 53 Controlling the ELSD within OpenLab CDS OpenLab ChemStation or OpenLab EZChrom 54 General Considerations 55 Solvent Recommendations...

Страница 42: ...t 1260 Infinity II ELSD G4260B or the Agilent 1290 Infinity II ELSD G7102A either Serial or LAN must be selected as the method of communication If Serial communication is selected then no further configuration is required If LAN communication is selected further configuration of the network settings is required see chapter LAN Configuration ...

Страница 43: ...method status evaporator temperature nebulizer 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 Keypad 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 ...

Страница 44: ...the desired option is flashing Using the up down arrow keys to alter the parameter to the desired setting 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 ...

Страница 45: ...creen allows changes to the following electronic parameters Figure 8 G4260B submenu screen Figure 9 G7102A submenu screen Pmt Set Signal Gain Smth Set Time Constant LED Set Light Source Intensity PwrMd Set Mode of ELSD when powered up HZ Set Data Output Rate LAN Displays the instruments TCP IP settings With serial connection option displays Instrument Configured for RS 232 ...

Страница 46: ...ore switching the unit into RUN mode The instrument will default to STANDBY mode should an error occur on the instrument Following a command or error the instrument is switched from RUN to STANDBY mode In this situation 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 STANDBY enough...

Страница 47: ...he heaters light source and gas are turned off A complete list of instrument errors and remedial actions is given in the troubleshooting section of this manual 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 CAUTION Solve...

Страница 48: ...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 corner These on board methods cannot be edited Evaporator Temperature The evaporator temperature is the most important setting on the ELS detector It should be set according to the volatility of the compounds being analyzed...

Страница 49: ...le phase composition Likewise as the evaporator temperature is reduced to ambient and subambient 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 no...

Страница 50: ... This feature is useful for preparative chromatography where samples of high concentration can be analyzed which would otherwise exceed the dynamic range of the detector Power Mode The instrument can be configured from the front panel submenu see Submenu Screen on page 45 to start in either RUN or STANDBY mode when the unit is switched on via the rear power button To configure the Power Mode selec...

Страница 51: ...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 LAN TCP IP Settings This screen displays the ELSD s current configured TCP IP settings See chapter LAN Configuration for details on how to set these values With serial connection screen option displays Instrument Configure...

Страница 52: ... can be purchased from Agilent ELSD Dimension Software includes trigger cable PL0890 0375 A trigger cable has to be ordered separately Use Infinity II Trigger Cable for Dimension Software G4260 63002 for an Infinity II system and Remote start cable PL0890 0350 for a third party system Creating a Real Time Program To create or modify the onboard timetable the ELSD Dimension software must be install...

Страница 53: ...e current and the total run time are displayed 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 behavior is normal ba...

Страница 54: ...nLab CDS OpenLab ChemStation ChemStation Rev B not supported or OpenLab EZChrom 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 ELS...

Страница 55: ...cessary The intended eluent should be thoroughly degassed should not contain nonvolatile salts or material and should be fully compatible with the columns All connections should be made with zero dead volume fittings and tubing with an I D 0 254 mm 0 010 in The ELSD requires nitrogen of purity 98 at an inlet pressure of 4 1 6 9 bar 60 100 psi If in house nitrogen is not available we recommend the ...

Страница 56: ...F should be used with the ELS detector Solvents with high boiling points such as N methylpyrrolidone NMP Dimethylsulphoxide DMSO m Cresol and 1 2 4 Trichlorobenzene TCB are not recommended Sample Preparation Samples containing particulate matter should be filtered through a 0 45 µm filter prior to injection Column Considerations The ELS detector will detect all nonvolatile components in the mobile...

Страница 57: ... Acetic Acid 4 75 9 25 116 0 16 6 Bases Ammonia 9 25 4 75 33 4 77 7 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 9 2 3 0 5 0 8 2 10 2 120 Ammonium Acetate 4 8 9 2 3 8 5 8 8 2 10 2 111 Ammonium Bicarbonate 6 3 9 2 10 3 6 8 11 3 106 Ion Pair Reagent Pentafluoropropionic acid PFPA 0 6 97 Heptafluorobutyric acid HFBA 0...

Страница 58: ...ctor 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 G7102A can be operated as low as 20 30 C for the equivalent solvent Therefore the transfer of operating conditions from other model...

Страница 59: ...anual 59 5 Optimizing Performance Do s and Don ts of ELS Detection 60 Location of the Detector Module 61 Pumping Systems 62 Mobile Phase Priming 63 This chapter gives hints on how to optimize the performance or use additional devices ...

Страница 60: ... performance High pressures on the internal chamber will lead to increased baseline noise and low sensitivity NEVER block the exhaust outlet NEVER allow the solvent waste outlet tube to become immersed in the waste solvent When placing more than one HPLC detector in series always place the ELS detector last Only use volatile mobile phase additives ...

Страница 61: ...e length of the power cord fluid lines and signal cables 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 10 cm 4 inches 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 de...

Страница 62: ...g 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 to minimize pulsation This can also be achieved by the column itself or a coil of 0 127 mm 0 005 in ID tubing placed between the pump and the injector injection valve ...

Страница 63: ...etector does not require any mobile phase priming It is recommended that priming of the LC system is performed without the ELS detector attached to prevent nonvolatile impurities contaminating the ELS detector The mobile phase should be degassed and filtered either by sparging with Helium or using an online degasser ...

Страница 64: ...Fails to zero 70 No power 70 No response completely flat baseline 71 Temperature error as soon as instrument powered on 71 Display not on but power connected 72 Cooled Evaporator Temperature reads zero at start up and cannot be changed 72 Vapor sensor error occurs but there is no solvent or vapor leak inside unit 72 Cooled Evaporator will not reach low temperature e g 10 C 73 High backpressure fro...

Страница 65: ...rces The ELS Detector itself can be dirty or operating outside specification The HPLC system has a broken dirty or nonoptimally operating component but the problem is manifesting itself in the ELS Detector A mobile phase and or column problem which by its very nature is spread throughout the HPLC system but appears as a malfunction of the ELS Detector To troubleshoot the ELS Detector you must be a...

Страница 66: ...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 re occurs 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 ...

Страница 67: ...low rate Decrease the nebulization temperature 3 Nonvolatile additive in mobile phase Use a volatile mobile phase 4 Pressure difference created inside nebulizer chamber 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 5 Pump pulsations especially in MicroBore applications where low flow ra...

Страница 68: ...reases 5 Nonvolatile additive in mobile phase Use a volatile mobile phase Probable cause Suggested actions 1 Partial blockage in nebulizer or nebulizer inlet tube Pump a 50 50 water acetone mixture into ELSD at highest flow rate possible do not exceed 5 mL min for 16 h 2 Internal solvent trap is empty Fill the front solvent trap with liquid until any excess flows out through front drain tube 3 Gas...

Страница 69: ...he 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 Probable cause Suggested actions 1 Inef...

Страница 70: ...aration Probable cause Suggested actions 1 Offset too high or output unstable due to impurity in mobile phase Stop pump flow and switch off unit Restart unit and A Z without liquid flowing Refer to local distributor or Agilent Technologies Optical section contaminated and requires cleaning Probable cause Suggested actions 1 Mains lead not connected Attach mains lead to socket and inlet on rear of ...

Страница 71: ... 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 should be below 130 mV 3 Output below 0 mV Stop pump flow and A Z without liquid flowing 4 Instrument in STANDBY mode Select RUN mode 5 Nebulizer or nebulizer inlet tube blocked Manually syringe water into ELSD front Inlet port to remove obstruction Pro...

Страница 72: ...distributor or Agilent Technologies 2 Faulty display Refer to local distributor or Agilent Technologies 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 Probable cause Suggested actions 1 Solvent vapor near the front of unit is being drawn into the unit ...

Страница 73: ...or Probable cause Suggested actions 1 Ambient lab temperature too high Move detector to laboratory where ambient temperature is 25 C 2 Faulty Peltier cooler unit Consult Agilent Technologies or your local agent if problem persists Probable cause Suggested actions 1 Nebulizer or nebulizer inlet tube blocked Manually syringe water into ELSD front Inlet port to remove obstruction ...

Страница 74: ...temperature limit exceeded 79 LED or Laser light source error 79 Evaporator gas flow rate limit exceeded 79 Invalid Nebulizer temperature 80 Invalid Evaporator temperature 80 Fan failed on cooled evaporator 80 Cooled evaporator current out of range or communication failed 81 Laser temperature out of range 81 Laser current out of range 81 Laser interlock open or failed 82 Communication to Laser fai...

Страница 75: ...r 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 ELSD alarms with an error message displayed ...

Страница 76: ...s failed Probable cause Suggested actions 1 The environmental temperature is outside the specified operating limits of the instrument Increase ambient temperature where detector is located Move the detector to a warmer location Probable cause Suggested actions 1 The environmental temperature is outside the specified operating limits of the instrument Decrease ambient temperature where detector is ...

Страница 77: ...your Agilent service representative 2 Defective vapor sensor Please contact your Agilent service representative Probable cause Suggested actions 1 External vapor being drawn into unit Remove any source of solvent vapors close to the module 2 Solvent leak inside unit Please contact your Agilent service representative 3 Exhaust tube not fitted Fit black exhaust tube Probable cause Suggested actions ...

Страница 78: ...ective fan Please contact your Agilent service representative 3 Defective mainboard Please contact your Agilent service representative Probable cause Suggested actions 1 Obstruction of fan blades Please contact your Agilent service representative 2 Defective fan Please contact your Agilent service representative 3 Defective mainboard Please contact your Agilent service representative Probable caus...

Страница 79: ...vice representative 2 Defective evaporator heater assembly Please contact your Agilent service representative 3 Defective mainboard Please contact your Agilent service representative Probable cause Suggested actions 1 LED or Laser Light source not connected to the mainboard Please contact your Agilent service representative 2 Defective LED or Laser Light source Please contact your Agilent service ...

Страница 80: ...ent service representative 2 Defective nebulizer heater Please contact your Agilent service representative Probable cause Suggested actions 1 Evaporator heater not connected to the mainboard Please contact your Agilent service representative 2 Defective evaporator heater Please contact your Agilent service representative 3 RTD Block to TEC board for cooled ELSD not connected to the mainboard Ensur...

Страница 81: ...rrent out of range Error ID 27 Laser current outside of normal operating range Probable cause Suggested actions 1 Defective Peltier assembly Please contact your Agilent service representative 2 Peltier assembly not connected to mainboard Please contact your Agilent service representative 3 Defective mainboard Please contact your Agilent service representative Probable cause Suggested actions 1 Def...

Страница 82: ...ur Agilent service representative 3 Interlock wiring is faulty Please contact your Agilent service representative 4 Defective mainboard Please contact your Agilent service representative Probable cause Suggested actions 1 Laser assembly not connected to mainboard Please contact your Agilent service representative 2 Defective Laser assembly Please contact your Agilent service representative 3 Defec...

Страница 83: ...nance 84 Cautions and Warnings 85 Cleaning the Module 87 Inspection of Cables 88 Drying the Diffuser 89 Cleaning the Nebulizer 90 Cleaning Evaporator Tube 91 Putting the Instrument into Storage 92 Updating Detector Firmware 93 This chapter describes the maintenance of the ELSD ...

Страница 84: ...rsonnel 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 Information for Service Personnel Please note that this instrument is double fused The following fuses are fitted 2x T2A H 250 V ...

Страница 85: ... solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks When working with these substances observe appropriate safety procedures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice The volume of substances shou...

Страница 86: ...lay etc are used for replacement 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 ESD can damage electronic boards and components 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 handli...

Страница 87: ...th a cloth moistened with de ionized 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 Switch off and disconnect power cord from instrument before cleaning Do not use an excessively damp cloth during cleaning Drain all solvent lines before opening any fittings Allow the instrument to ...

Страница 88: ...finityLab ELSD User Manual 88 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 ...

Страница 89: ...increased baseline noise and in the extreme case gas bubbling out of the nebulizer 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 sta...

Страница 90: ...eading to the nebulizer To clean the nebulizer the following procedure is recommended 1 Put the ELSD into RUN mode 2 Set the evaporator and nebulizer temperature to 40 C and the gas flow to 1 6 SLM 3 Set pump flow rate to 5 mL min 4 Remove the column select a suitable solvent for example water if using aqueous buffers and pump for 3 h or set pump flow rate to 1 mL min and run overnight NOTE Pump t...

Страница 91: ...0 h of use as a preventive routine It is also recommended to clean the unit following the use of buffers If cleaning the unit does not solve the problems consult Agilent Technologies for further assistance 1 Set the evaporator temperature to 40 C the nebulizer temperatures to 40 C and the gas flow to 2 8 SLM 2 Pump the cleaning solvent into the instrument at 1 2 mL min while in the RUN mode overni...

Страница 92: ... 3 Tip the instrument forwards to try and empty the solvent within the nebulization chamber through the front waste tube i e into the bottle 4 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 5 Repeat step 3 to drain the acetone 6 Disconnect the waste bottle 7 Using the gas supply blow nitrogen g...

Страница 93: ... using the same process Firmware upgrade is only possible via the serial port 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 RS 232 cable 2 Open the Tera Term program and select File New Connection from the toolbar When For majority of internal repairs Tools required Description Allen keys...

Страница 94: ...followed by OK 4 From the toolbar menu select Setup Serial Port to configure the serial port connection 5 Set the Serial port to the parameters shown below and click OK The Transmit delay values should be set according to the table below Table 11 Transmit delay values Firmware type msec char msec line Main 0 20 Safety 0 35 Laser 0 35 ...

Страница 95: ...hilst switching on the module The front panel will display SERVICE MODE Reboot for normal operation When in Service mode the Tera Term displays the bootloader version and firmware menu 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 ...

Страница 96: ...elect the Send File option from the File menu in the toolbar and navigate to the folder where the file is located 10 Select the firmware hex file and click Open The download will begin straightaway and progress will be displayed as shown NOTE Do not disconnect or turn off the detector during the transfer process ...

Страница 97: ... Updating Detector Firmware 11 On successful completion of the file transfer the software will display a Flash memory updated ok message 12 Power cycle the module and check that the firmware version displayed on the ELSD front panel at boot up is correct ...

Страница 98: ...Agilent InfinityLab ELSD User Manual 98 9 Parts and Materials for Maintenance Identifying Parts and Materials 99 This chapter provides information on parts for maintenance ...

Страница 99: ...let tube 5 m PL0890 0310 A Rear exhaust hose PVC 2 m PL0890 0315 A Solvent waste tube 2 m PL0890 0325 A RS232 communication cable G4260 63001A Infinity II Modules to ELSD Trigger Cable G4260 63002 A Infinity II Trigger Cable for Dimension Software PL0890 0640 A ELSD Air Adapter Kit 8121 0008A LAN shielded cable G4260 60005 A 1260 1290 ELSD Infinity I Trigger Cable PL0890 0350 A Remote start cable ...

Страница 100: ...l 100 10 Appendix General Safety Information 101 Waste Electrical and Electronic Equipment WEEE Directive 105 Radio Interference 106 Agilent Technologies on Internet 107 This chapter provides addition information on safety legal and Web ...

Страница 101: ...ted up Sample Cooler unit is designed as vapor compression refrigeration system Contains fluorinated greenhouse gas refrigerant according to the Kyoto protocol For specifications of refrigerant charge capacity carbon dioxide equivalent CDE and global warming potential GWP see instrument label Flammable Material For Sample Thermostat which uses flammable refrigerant consult Agilent Information Cent...

Страница 102: ... from getting too close to magnets Magnetic field Magnets produce a far reaching strong magnetic field They could damage TVs and laptops computer hard drives credit and ATM cards data storage media mechanical watches hearing aids and speakers Keep magnets at least 25 mm away from devices and objects that could be damaged by strong magnetic fields Indicates a pinching or crushing hazard Indicates a...

Страница 103: ...s of design manufacture and intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements 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 WARNING Ensure the proper usage of the equipment The prot...

Страница 104: ... 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...

Страница 105: ...ective This product complies with the European WEEE Directive marking requirements The affixed label indicates that you must not discard this electrical electronic product in domestic household waste NOTE Do not dispose of in domestic household waste To return unwanted products contact your local Agilent office or see https www agilent com for more information ...

Страница 106: ...Interference Agilent InfinityLab ELSD User Manual 106 Radio Interference Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations ...

Страница 107: ... ELSD User Manual 107 10 Appendix Agilent Technologies on Internet Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at https www agilent com ...

Страница 108: ...tion on the Agilent 1260 Infinity II Evaporative Light Scattering Detector G4260B and Agilent 1290 Infinity II Evaporative Light Scattering Detector G7102A The manual describes the following Introduction Site Requirements and Specifications Using Optimizing Troubleshooting and Diagnostics Error Information Maintenance Parts Safety ...

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