Agilent Technologies 1260 Infinity II Refractive Index Detector User Manual Download Page 103

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Agilent InfinityLab LC Series RID User Manual

103

Test Functions

Introduction

104

Refractive Index Calibration

108

Optical Balance

114

The Optical Balance Procedure

115

Using the Build-in Test Chromatogram

117

Procedure Using the Agilent LabAdvisor

117

ASTM Drift and Noise Test

119

Setting the Test Conditions

119

Evaluation

122

D/A Converter (DAC) Test

123

Test Evaluation

124

Other Lab Advisor Functions

125

EMFs - Early Maintenance Feature

125

This chapter describes the detector’s built in test functions.

Summary of Contents for 1260 Infinity II Refractive Index Detector

Page 1: ...Refractive Index Detector Agilent InfinityLab LC Series User Manual Agilent InfinityLab LC Series RID User Manual ...

Page 2: ...in this document that conflict with these terms the warranty terms in the separate 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 fed...

Page 3: ...fications 3 Using the Module This chapter explains the essential operational parameters of the module 4 Preparing the Module This chapter provides information on how to set up the module for an analysis and explains the basic settings 5 Optimizing the Detector This chapter provides information on how to optimize the detector 6 Troubleshooting and Diagnostics This chapter gives an overview about th...

Page 4: ...e This chapter provides information on parts for maintenance 11 Identifying Cables This chapter provides information on cables used with the Agilent 1200 Infinity Series modules 12 Hardware Information This chapter describes the module in more detail on hardware and electronics 13 LAN Configuration This chapter provides information on connecting the module to the Agilent ChemStation PC 14 Appendix...

Page 5: ...Handling 27 2 Site Requirements and Specifications 33 Site Requirements 34 Physical Specifications 37 Performance Specifications 38 3 Using the Module 42 Magnets 43 Turn on off 44 Status Indicators 46 Instrument Configuration 47 Set up the Detector with Agilent Open Lab ChemStation 49 The Detector User Interface 50 Detector Control Settings 53 Method Parameter Settings 55 Agilent Local Control Mod...

Page 6: ...rror Messages 94 Not Ready Messages 101 8 Test Functions 103 Introduction 104 Refractive Index Calibration 108 Optical Balance 114 Using the Build in Test Chromatogram 117 ASTM Drift and Noise Test 119 D A Converter DAC Test 123 Other Lab Advisor Functions 125 9 Maintenance and Repair 126 Introduction to Maintenance 127 Warnings and Cautions 128 Overview of Maintenance 130 Cleaning the Module 131 ...

Page 7: ...59 12 Hardware Information 160 Data Flow for Chromatographic Output 161 Firmware Description 162 Electrical Connections 165 Interfaces 168 Setting the 6 bit Configuration Switch 176 Instrument Layout 180 Early Maintenance Feedback 181 13 LAN Configuration 182 What You Have to Do First 183 TCP IP parameter configuration 184 Configuration Switches 185 Initialization Mode Selection 186 Dynamic Host C...

Page 8: ...ser Manual 8 In This Guide 14 Appendix 204 General Safety Information 205 Waste Electrical and Electronic Equipment WEEE Directive 211 Radio Interference 212 Sound Emission 213 Solvent Information 214 Agilent Technologies on Internet 216 ...

Page 9: ...162A Refractive Index Detector 12 Product Description 12 Features 13 G7162B Refractive Index Detector 14 Product Description 14 Features 15 How the Detector Operates 16 Detection Principle 18 Flow Path 20 Leak and Waste Handling 27 Leak Sensor 31 Waste Guidance 31 Waste Concept 32 This chapter gives an introduction to the Refractive Index Detector ...

Page 10: ... optics ready to use within two hours of installation automatic zero and automatic purge combined with a recycle valve for automatic solvent recycling allow uninterrupted operation durable tungsten lamp with a life expectancy of 40000 hours automatic light intensity control circuit to ensure the optimum performance of the optics integrated diagnostics for efficient troubleshooting built in refract...

Page 11: ...for all standard applications It comprises the following features inlet port to sample cell 62 µL inlet port to outlet port 590 µL maximum data rate up to 74 Hz G7162B Refractive Index Detector Micro This detector is equipped with the micro optical unit and is used for all low volume applications It comprises the following features inlet port to sample cell 10 µL inlet port to outlet port 265 µL m...

Page 12: ...fractive Index Detector RID is the ideal detector for fast and reliable LC results when routinely analyzing non UV absorbing substances such as carbohydrates lipids and polymers The 1260 Infinity II RID is also the detector of choice for gel permeation chromatography GPC or size exclusion chromatography SEC Figure 2 Overview of the detector Status indicator Interface port area Service door Power s...

Page 13: ...between runs Programmable reference cell purging autopurge and auto zeroing of the detector baseline before each run for unattended operation Convenient front access to the flow connections and valves next to the optical unit Early Maintenance Feedback EMF for prior notification of detector maintenance and continuous tracking of reference flow cell purging with user settable limits Fast and simple...

Page 14: ...with an ultralow dispersion microflow cell which significantly reduces run times for higher sample throughput and improved resolution Lower solvent consumption means much lower cost of analysis A high performance detector of choice for accurate reproducible routine analysis of polymers and other compounds that aren t detectable by UV Figure 3 Overview of the detector Status indicator Interface por...

Page 15: ...rately quantified Minimized band broadening high definition sample profiling Fast startup advanced low thermal mass design means that initial setup is typically less than two hours Further time and solvent saving a recycle valve enables sample to be recirculated when the sample is not passing through the flow cell Automatic purging of reference flow cell using programmable purge and wait times Eas...

Page 16: ...velocity and direction changes The change in direction is called refraction The relationship between the angle of incidence and the angle of refraction is expressed in Snell s Law of refraction Where n Refractive index of medium 1 relative to medium 2 n2 Refractive index of medium 2 n1 Refractive index of medium 1 α1 angle of incident light in medium 1 α2 angle of refraction in medium 2 Figure 4 L...

Page 17: ...ive index of medium 1 Factors that Affect Refractive Index The refractive index of a medium is affected by a number of factors 1 Wavelength The refractive index varies with changes in the wavelength of the incident light beam 2 Density As the density of the medium changes the refractive index changes At a fixed wavelength of incident light the changes in refractive index are generally linear in re...

Page 18: ...n the liquids in the sample and reference cells of a single flow cell A beam of light from the lamp passes through a flow cell which is separated diagonally into sample and reference cells At the rear of the flow cell a mirror reflects the light back through the flow cell and via a zero glass which affects the path of the light beam to the light receiver The light receiver has two diodes each of w...

Page 19: ...ample elutes from the column into the sample cell the refractive index of the cell contents changes The change in refractive index deflects the light beam as it passes through the flow cell resulting in an unequal amount of light falling on each diode The change in current from the diodes that this causes is amplified and used to produce the calibrated detector signal This signal expressed as nano...

Page 20: ... analysis starts Using this mode provides the benefits of uninterrupted flow through the detector without the problems of excessive solvent usage or the contamination of mobile phase with recycled sample compounds If the purge valve is in the on position the eluent cannot pass immediately to the recycle valve but will instead flow via a second heat exchanger through the reference cell and then int...

Page 21: ...n to the Refractive Index Detector Flow Path Normal Flow Mode Purge Valve OFF Recycle Valve OFF Mirror Sample cell Reference cell Heater Collimator lens Zero glass Diodes Slit lens Lamp Purge valve valve Recycle Safety cap Interconnection Heat exchanger Condenser ...

Page 22: ...urge Mode This mode is used for flushing the complete detector inclusive the reference side of the flow cell Purge Valve ON Recycle Valve OFF Mirror Sample cell Reference cell Heater Collimator lens Zero glass Diodes Slit lens Lamp Purge valve valve Recycle Safety cap Interconnection Heat exchanger Condenser ...

Page 23: ...ath Recycle Mode This mode is used for saving solvent during periods where no sample is running through Purge Valve OFF Recycle Valve ON Mirror Sample cell Reference cell Heater Collimator lens Zero glass Diodes Slit lens Lamp Purge valve valve Recycle Safety cap Interconnection Heat exchanger Condenser ...

Page 24: ...o reference cell 3 2 4 to optical unit sample cell bottom right Metal union block Recycle valve NC NO NC NO COM COMMON NO NORMALLY OPEN NC NORMALLY CLOSED C ON N E C T I N G P O R T S COM WASTE IN COM RECYCLE Capillaries 1 to 4 are part of the optical unit assembly They are made of SST with an ID of 1 0 mm except for 2 which has an ID of 0 2 mm All other tubings to and from the purge and the refer...

Page 25: ...FF COM COM NO NC NO NC Metal union block Sample cell Reference cell WASTE RECYCLE Purge valve Recycle valve COM COMMON NO NORMALLY OPEN NC NORMALLY CLOSED IN Grey lines flowing path Black lines immobilized mobile phase The T connection in the metal union block results in both sides of the flow cell sample and reference always being exposed to the same pressure ...

Page 26: ...N NO NC COM Purge valve Recycle valve COM NC NO Metal union block Sample cell Reference cell WASTE RECYCLE IN COM COMMON NO NORMALLY OPEN COM NORMALLY CLOSED Grey lines flowing path Black lines immobilized mobile phase The T connection in the metal union block results in both sides of the flow cell sample and reference always being exposed to the same pressure ...

Page 27: ... Internet All leak plane outlets are situated in a consistent position so that all Infinity and Infinity II modules can be stacked on top of each other Waste tubes are guided through a channel on the right hand side of the instrument keeping the front access clear from tubes The leak plane provides leak management by catching all internal liquid leaks guiding them to the leak sensor for leak detec...

Page 28: ...Agilent InfinityLab LC Series RID User Manual 28 1 Introduction to the Refractive Index Detector Leak and Waste Handling Figure 10 Infinity II Leak Waste Concept Flex Bench installation ...

Page 29: ...Agilent InfinityLab LC Series RID User Manual 29 1 Introduction to the Refractive Index Detector Leak and Waste Handling Figure 11 Infinity II Single Stack Leak Waste Concept bench installation ...

Page 30: ...ion to the Refractive Index Detector Leak and Waste Handling Figure 12 Infinity II Two Stack Leak Waste Concept bench installation The waste tube connected to the leak pan outlet on each of the bottom instruments guides the solvent to a suitable waste container ...

Page 31: ...patibility The solvent DMF dimethyl formamide leads to corrosion of the leak sensor The material of the leak sensor PVDF polyvinylidene fluoride is incompatible with DMF Do not use DMF as mobile phase Check the leak sensor regularly for corrosion NOTE The waste drainage must go straight into the waste containers The waste flow must not be restricted at bends or joints ...

Page 32: ...with 4 ports 5043 1221 for optimal and safe waste disposal If you decide to use your own waste solution make sure that the tubes don t immerse in the liquid NOTE To optimize detector performance the waste container and solvent bottle should be positioned above the level of the refractive index detector and solvent pump e g in the solvent compartment This will maintain a slight pressure in the samp...

Page 33: ...User Manual 33 2 Site Requirements and Specifications Site Requirements 34 Physical Specifications 37 Performance Specifications 38 This chapter provides information on environmental requirements physical and performance specifications ...

Page 34: ...the devices are connected to a line voltage higher than specified Connect your instrument to the specified line voltage only WARNING Electrical shock hazard The module is partially energized when switched off as long as the power cord is plugged in The cover protects users from personal injuries for example electrical shock Do not open the cover Do not operate the instrument and disconnect the pow...

Page 35: ...oses can lead to personal injury or damage of electronic equipment Never use a power cord other than the one that Agilent shipped with this instrument Never use the power cords that Agilent Technologies supplies with this instrument for any other equipment Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulati...

Page 36: ...e conditions 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 hour 1 8 F hour Turbulences around one minute or less can be ignored NOTE Agilent recommends that you install the HPLC instru...

Page 37: ... 1 x 15 6 x 17 2 inches Line voltage 100 240 V 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 80 VA 70 W Ambient operating tempera ture 4 55 C 39 131 F Ambient non operating tem perature 40 70 C 40 158 F Humidity 95 r h at 40 C 104 F Non condensing Operating altitude Up to 3000 m 9842 ft Safety standards IEC EN CSA UL Installation category II Pollution degree 2 For indoo...

Page 38: ... rate 5 mL min Valves Automatic purge and automatic solvent recycle Volumes Inlet port to sample cell 62 µL inlet port to outlet port 590 µL Liquid contact materials 316 stainless steel PTFE and quartz glass pH range 2 3 9 5 Performance specifications Short term noise 1 25 10 9 RIU Drift 200 10 9 RIU hr Time programmable param eters Polarity peak width Maximum data rate 74 Hz Detector zero Automat...

Page 39: ...essages Elec tronic records of maintenance and errors Automated operational qualification performance verification OQ PV Housing All materials recyclable Table 2 Agilent 1260 Infinity II Refractive Index Detector G7162A Performance Specifications Type Specification NOTE Based on ASTM method E 1303 95 Practice for Refractive Index Detectors used in Liquid Chromatography Reference conditions optics ...

Page 40: ...le cell 2 5 µL inlet port to outlet port 265 µL Liquid contact materials 316 stainless steel PTFE and quartz glass pH range 2 3 9 5 Performance specifications Short term noise 1 75 10 9 RIU Drift 200 10 9 RIU hr Time programmable param eters Polarity peak width Maximum data rate 148 Hz Detector zero Automatic zero before analysis Instrument Control Lab Advisor B 02 07 or above LC and CE Drivers A ...

Page 41: ...ce verification OQ PV Housing All materials recyclable Table 3 Agilent 1290 Infinity II Refractive Index Detector G7162B Performance Specifications Type Specification NOTE Based on ASTM method E 1303 95 Practice for Refractive Index Detectors used in Liquid Chromatography Reference conditions optics temperature 35 C response time 4 s flow 1 0 mL min LC grade Water restriction capillary column comp...

Page 42: ...atus Indicators 46 Instrument Configuration 47 Set up the Detector with Agilent Open Lab ChemStation 49 The Detector User Interface 50 Detector Control Settings 53 Method Parameter Settings 55 Agilent Local Control Modules 59 This chapter explains the essential operational parameters of the module ...

Page 43: ...Agilent InfinityLab LC Series RID User Manual 43 3 Using the Module Magnets Magnets 1 Magnets in doors of pumps autosamplers detectors and fraction collectors ...

Page 44: ...Agilent InfinityLab LC Series RID User Manual 44 3 Using the Module Turn on off Turn on off This procedure exemplarily shows an arbitrary LC stack configuration 1 2 Power switch On ...

Page 45: ...Agilent InfinityLab LC Series RID User Manual 45 3 Using the Module Turn on off 3 Turn instrument On Off with the control software 4 Power switch Off 5 ...

Page 46: ...ossible module conditions Status indicators 1 Idle 2 Run mode 3 Not ready Waiting for a specific pre run condition to be reached or completed 4 Error mode interrupts the analysis and requires attention for example a leak or defective internal components 5 Resident mode blinking for example during update of main firmware 6 Bootloader mode fast blinking Try to re boot the module or try a cold start ...

Page 47: ...figuration Instrument Configuration 1 Set the switches of the Configuration switch at the rear of the module a All switches DOWN module uses the default IP address 192 168 254 11 b Switch 4 UP and others DOWN module uses DHCP c Switch 5 UP and others DOWN modules uses STORED address ...

Page 48: ... RID User Manual 48 3 Using the Module Instrument Configuration 2 Enter the setup information MAC IP address and or Instrument Name a Agilent OpenLAB ChemStation Configure Instrument b Lab Advisor Instrument Overview Add Instrument ...

Page 49: ...penLab ChemStation C 01 07 and LC and CE Drivers A 02 13 Figure 13 ChemStation Method and Run Control just detector is shown After successful load of the OpenLab ChemStation you should see the module as an active item in the graphical user interface GUI NOTE This section describes the detector settings only For information on the Agilent OpenLab ChemStation or other 1200 Infinity modules refer to ...

Page 50: ...or GUI there are active areas If you move the mouse cursor across the icons the cursor will change 1 Make device ready or turn off 2 EMF status 3 Detector status 4 Balance 5 Heater status on off 6 Heater temperature The Purge Valve status closed open and the Recycle Valve status off on is shown when the cursor moves across the flow cell icon ...

Page 51: ...nterface displays the above status Module Status shows Run Ready Error state and Not Ready text or Error text Error red Not ready yellow Ready green Pre run Post run purple Run blue Idle green Offline dark gray Standby light gray A right click into the Active Area will open a menu to Show the Control Interface special module settings Show the Method interface similar as via menu Instru ment Setup ...

Page 52: ...Agilent InfinityLab LC Series RID User Manual 52 3 Using the Module The Detector User Interface If the Purge Valve or Recycle Valve has been turned on the on time is displayed below the flow cell icon ...

Page 53: ...eter requires setting the Optical Unit Temperature Select the Off option to switch the optical unit heater off Analog Output Range can be set to either 100 mV or 1 V full scale for additional settings see Analog Output under Method Parameter Settings on page 55 At Power On When activated the optical unit heater is turned on automatically when the RID is switched on For shortest equilibration times...

Page 54: ... if you click OK on this window Allow additional time for baseline stabilization after purging Recycling Valve Select the On option to switch the recycling of the eluent on The Off option diverts the flow of the RID to the waste bottle Automatic Turn On This function allows you to turn on the optical unit heater at a specified date and time It requires that the At Power On function is turned off S...

Page 55: ...vailable via Menu Instrument Set up Instrument Method or via right click into the module s active area does not show the Instrument Curves tab Figure 15 Method parameter settings NOTE For additional help and support Highlight the desired cell and press F1 A help screen will open with additional information and documentation about the topic ...

Page 56: ...e time is set automatically and the appro priate data rate for signal acquisition is selected If Acquire Signal check box is not marked signals are not stored NOTE The 1260 Infinity II RID G7162A has a data rate of up to 74 Hz The 1290 Infinity II RID G7162B has a data rate of up to 148 Hz Stoptime Posttime The Stoptime is the time where either the complete system stops As Pump Injector or the mod...

Page 57: ...irecting the effluent to the waste outlet of the RID Off after the run Automatic Purge This parameter can be used to purge the reference cell and wait additional time for baseline stabilization It is initiated each time the run is started This should be used only if the content of the reference cell is expected to degrade during a run The automatic purge is completed before the autozero is perform...

Page 58: ...ature Diode Balance to diagnose peaks that exceed the dynamic range of the RID for example in the case of extremely high concentrations signals Polarity monitors of polarity switching during the run Diode 1 and Diode 2 The RID signal is based on the ratio of the light level that is measured by two photodiodes The RID signal is zero if the two diodes show the same light level This parameter allows ...

Page 59: ... of Agilent Infinity II Prime LC Modules Excellent usability and ease of use through a user interface specifically tailored for mobile devices simple intuitive touch enabled and visual controllable High flexibility through a modern Bring your own device approach Connection between LC module and mobile device either wireless via WLAN or wired over USB cable with full package Convenient ergonomic op...

Page 60: ...00 Series 1200 Series SL and 1100 Series Excellent readability and usability by large colored display with background light high resolution and contrast Convenient ergonomic operation either handheld or at the stack with newly developed secure attachment Handheld or attached to a module in a stack to facilitate operator preferences The 1200 Infinity Series Instant Pilot provides Easy automation re...

Page 61: ...etting up an Analysis 64 Before Using the System 65 Requirements and Conditions 66 Preparing the Detector 69 Preparing the HPLC System 69 Running the Sample and Verifying the Results 71 Solvent Information 72 This chapter provides information on how to set up the module for an analysis and explains the basic settings ...

Page 62: ...s the solvent temperature in the sample compartment For the solvents methanol and ethanol keep the solvent temperature at least 25 K below the boiling point Do not operate the instrument in an explosive atmosphere Do not use solvents of ignition Class IIC according IEC 60079 20 1 for example carbon disulfide Reduce the volume of substances to the minimum required for the analysis Never exceed the ...

Page 63: ... 5043 1221 for optimal and safe waste disposal If you decide to use your own waste solution make sure that the tubes don t immerse in the liquid NOTE To optimize detector performance the waste container and solvent bottle should be positioned above the level of the refractive index detector and solvent pump e g in the solvent compartment This will maintain a slight pressure in the sample cell ...

Page 64: ...g up an Analysis This chapter can be used for preparing the system to learn the set up of an HPLC analysis and to use it as an instrument check to demonstrate that all modules of the system are correctly installed and connected It is not a test of the instrument performance Learn about special settings ...

Page 65: ... Priming Solvents for Different Purposes Activity Solvent Comments After an installation When switching between reverse phase and normal phase both times Isopropanol Isopropanol Best solvent to flush air out of the sys tem Best solvent to flush air out of the sys tem After an installation Ethanol or Methanol Alternative to Isopropanol second choice if no Isopropanol is available To clean the syste...

Page 66: ...is Some of these are optional not required for the basic system NOTE Pump for approximately 10minutes before starting your application NOTE Do NOT exceed the flow rate of the 1290 Infinity II RID Micro whilst purging pump Bypass detector when purging 1 mL min Table 6 What you will need Agilent 1200 Infinity Series system Pump plus degassing Autosampler Detector Degasser optional Column Compartment...

Page 67: ...t standard is made under the conditions given in Table 7 on page 67 Table 7 Chromatographic conditions Mobile phases 30 water 70 acetonitrile Flow rate 1 5 mL min Stroke A 20 µL Stop time 10 min Injection volume 20 µL Column compartment temperature 25 C Optical unit Temperature 35 C Polarity Positive Peak Width Response time 0 2 min 4 s standard ...

Page 68: ...The resulting chromatogram should only be seen as a qualitative example the checkout procedure is not meant as a quantitative procedure Its intent is only to verify the presence of the four peaks from the checkout sample Please be aware of the large negative air solvent peak from the injection cut out from the bottom of the following figure prior to the first peak of interest This is to be expecte...

Page 69: ...anel is removed while the TCC is set to high temperatures the up streaming air could influence the stability of the detector baseline Preparing the HPLC System 1 Turn on the control software and the monitor 2 Turn on the modules 3 Start the control software The screen should show all modules and the system status is Not Ready 4 Turn on the modules that require conditioning a Detector heater warm u...

Page 70: ...b LC Series RID User Manual 70 4 Preparing the Module Setting up an Analysis 7 Select the menu item Run Control Sample Info and enter information about this application Click OK to leave this screen Figure 17 Sample Info ...

Page 71: ...up an Analysis Running the Sample and Verifying the Results 1 To start a run select the menu item RunControl Run Method 2 This will start the modules and the online plot on the Agilent ChemStation will show the resulting chromatogram Figure 18 Isocratic standard sample chromatogram ...

Page 72: ...robustness under typical HPLC conditions For any special condition please consult the material information section or contact Agilent Disclaimer Subsequent data was collected from external resources and is meant as a reference Agilent cannot guarantee the correctness and completeness of such information Data is based on compatibility libraries which are not specific for estimating the long term li...

Page 73: ...d ensures pressure stability to at least 600 bar If in doubt consult the available literature about the chemical compatibility of PEEK Polyimide Agilent uses semi crystalline polyimide for rotor seals in valves and needle seats in autosamplers One supplier of polyimide is DuPont which brands polyimide as Vespel which is also used by Agilent Polyimide is stable in a pH range between 1 and 10 and in...

Page 74: ... acids like nitric acid sulfuric acid and organic solvents especially at higher temperatures replace if your chromatography method allows by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2 CHCl3 O2 2 COCl2 2 HCl This reaction in which stainless steel probably acts as a catalyst occu...

Page 75: ...nhydrous methanol which can be avoided by adding a small amount of water about 3 Slight corrosion is possible with ammonia 10 Diamond Like Carbon DLC Diamond Like Carbon is inert to almost all common acids bases and solvents There are no documented incompatibilities for HPLC applications Fused silica and Quartz SiO2 Fused silica is used in Max Light Cartridges Quartz is used for classical flow cel...

Page 76: ...tubings which are used in all Agilent degassers except G1322A G7122A are not compatible with fluorinated solvents like Freon Fluorinert or Vertrel They have limited life time in the presence of Hexafluoroisopropanol HFIP To ensure the longest possible life with HFIP it is best to dedicate a particular chamber to this solvent not to switch solvents and not to let dry out the chamber For optimizing ...

Page 77: ...eries RID User Manual 77 5 Optimizing the Detector Refractive Index Detector Optimization 78 Potential Causes for Baseline Problems 80 Detector Equilibration 81 This chapter provides information on how to optimize the detector ...

Page 78: ...e correct solvents To minimize baseline noise and drift solvents must be LC grade and filtered prior to use 4 Check for leaks Leaks within the LC instrument that the refractive index detector is connected to will cause problems with baseline long term noise or drift Confirm that the instrument is free from leaks by performing the diagnostic pressure test for the high pressure parts of the system b...

Page 79: ... analysis without wasting mobile phase solvents In addition the refractive index detector is always stabilized and ready for immediate use 9 Consider using a degasser For many solvents you can achieve better baseline stability when using a degasser For some solvents a degasser might not lead to a better baseline quality 10 Flush the degasser If flow is stopped and mobile phase remains inside the o...

Page 80: ... Baseline Problems Noise short term Typically the sources for short term noise are either electronic check the settings for the peak widths check for ambient sources of electronic noise or they are related to the solvents their composition and flow in order to verify this turn off the pump consider degassing your solvents use only premixed solvents Wander long term noise Excessive wander is an ind...

Page 81: ... the detector is often without justification blamed for instabilities which it does not generate itself but only detect The fact that this detector is a universal detector makes it also sensitive to instabilities introduced to it from outside the detector This makes it very important to have a very stable environment and system for achieving best possible baseline stability The baseline will get t...

Page 82: ... User Manual 82 6 Troubleshooting and Diagnostics Available Tests vs User Interfaces 83 Agilent Lab Advisor Software 84 This chapter gives an overview about the troubleshooting and diagnostic features and the different user interfaces ...

Page 83: ...terfaces NOTE Depending on the used interface the available tests and the screens reports may vary Preferred tool should be the Agilent Lab Advisor see Agilent Lab Advisor Software on page 84 Agilent Lab Advisor B 02 07 SP1 or later is required The Instant Pilot supports the G7162A B with B 02 19 or later It does not provide any test functions ...

Page 84: ... included with every Agilent 1200 Infinity Series and Agilent InfinityLab LC Series instrument The Lab Advisor Advanced features can be unlocked by purchasing a license key and include real time monitoring of instrument actuals all various instrument signals and state machines In addition all diagnostic test results calibration results and acquired signal data can be uploaded to a shared network f...

Page 85: ...oo High 94 Heater Fuse 95 Wrong Temperature Profile 95 Undecipherable Temperature Signal 96 Maximum Temperature Exceeded 96 Purge Valve Fuse Blown 97 Recycle Valve Fuse Blown 97 Purge Valve Not Connected 98 Recycle Valve Not Connected 98 Lamp Voltage too Low 99 Lamp Voltage too High 99 Lamp Current too High 99 Lamp Current too Low 100 Wait Function Timed Out 100 Not Ready Messages 101 Purge Time R...

Page 86: ...ification all LEDs get red and the run will be stopped Depending on the module type this stop is implemented differently For example for a pump the flow will be stopped for safety reasons For a detector the lamp will stay on in order to avoid equilibration time Depending on the error type the next run can only be started if the error has been resolved for example liquid from a leak has been dried ...

Page 87: ...d Probable cause Suggested actions 1 The analysis was completed successfully and the timeout function switched off the module as requested Check the logbook for the occurrence and source of a not ready condition Restart the analysis where required 2 A not ready condition was present during a sequence or multiple injection run for a period longer than the timeout threshold Check the logbook for the...

Page 88: ...Probable cause Suggested actions 1 Leak detected in an external instrument with a remote connection to the system Fix the leak in the external instrument before restarting the module 2 Shut down in an external instrument with a remote connection to the system Check external instruments for a shut down con dition 3 The degasser failed to generate sufficient vacuum for solvent degassing Check the va...

Page 89: ...hange within defined limits If the current falls outside the lower limit the error message is generated Probable cause Suggested actions 1 CAN cable disconnected Ensure all the CAN cables are connected cor rectly Ensure all CAN cables are installed correctly 2 Defective CAN cable Exchange the CAN cable 3 Defective mainboard in another module Switch off the system Restart the system and determine w...

Page 90: ... is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor increases above the upper limit the error message is generated Probable cause Suggested actions 1 Defective leak sensor Please contact your Agilent service representa tive 2 Leak sensor incorrectly routed being pinched by a meta...

Page 91: ...aft is used by the main board to monitor the fan speed If the fan speed falls below a certain limit for a certain length of time the error message is generated This limit is given by 2 revolutions second for longer than 5 seconds Depending on the module assemblies e g the lamp in the detector are turned off to assure that the module does not overheat inside Probable cause Suggested actions 1 Defec...

Page 92: ...ver Error ID 0205 The top foam has been removed The sensor on the main board detects when the top foam is in place If the foam is removed the fan is switched off and the error message is generated Probable cause Suggested actions 1 Loose fittings Ensure all fittings are tight 2 Broken capillary Exchange defective capillaries 3 Leaking valve Exchange valve 4 Leaking flow cell Exchange optical unit ...

Page 93: ...foam removed the lamps are switched off and the error message is generated ERI Messages Error ID 11120 5 V 11121 25 V The ERI Enhanced Remote Interface provides two error events related to over current situations on the 5 V and 24 V lines Probable cause Suggested actions 1 The top foam was removed during operation Please contact your Agilent service representa tive 2 Foam not activating the sensor...

Page 94: ...e the set limit Probable cause Suggested actions 1 Heater cable disconnected Please contact your Agilent service representa tive 2 Defective main board Please contact your Agilent service representa tive 3 Defective thermal fuse Please contact your Agilent service representa tive Probable cause Suggested actions 1 Heater cable disconnected Please contact your Agilent service representa tive 2 Defe...

Page 95: ...e temperature does not increase at a sufficiently fast rate to reach the set point Probable cause Suggested actions 1 Short in heater circuit Powercycle the module 2 Defective main board Please contact your Agilent service representa tive 3 Defective heater Please contact your Agilent service representa tive Probable cause Suggested actions 1 Defective main board Please contact your Agilent servic...

Page 96: ...en exceeded Probable cause Suggested actions 1 Heater cable disconnected Please contact your Agilent service representa tive 2 Defective main board Please contact your Agilent service representa tive 3 Defective heater Please contact your Agilent service representa tive Probable cause Suggested actions 1 Defective main board Please contact your Agilent service representa tive 2 Defective heater Pl...

Page 97: ...as been activated Probable cause Suggested actions 1 Short in purge valve circuit Power cycle the module 2 Defective purge valve Please contact your Agilent service representa tive 3 Defective main board Please contact your Agilent service representa tive Probable cause Suggested actions 1 Short in recycle valve circuit Power cycle the module 2 Defective recycle valve Please contact your Agilent s...

Page 98: ...robable cause Suggested actions 1 Purge valve disconnected Please contact your Agilent service representa tive 2 Defective purge valve Please contact your Agilent service representa tive 3 Defective main board Please contact your Agilent service representa tive Probable cause Suggested actions 1 Recycle valve disconnected Please contact your Agilent service representa tive 2 Defective recycle valv...

Page 99: ...ce representa tive 2 Defective lamp or optics Please contact your Agilent service representa tive Probable cause Suggested actions 1 Contaminated flow cell Flush the flow cell 2 Defective main board Please contact your Agilent service representa tive 3 Defective lamp or optics Please contact your Agilent service representa tive Probable cause Suggested actions 1 Defective main board Please contact...

Page 100: ...r wait for defined signal has not been fulfilled within the specified time frame Probable cause Suggested actions 1 Optical unit cable disconnected Please contact your Agilent service representa tive 2 Defective main board Please contact your Agilent service representa tive 3 Defective lamp or optics Please contact your Agilent service representa tive Probable cause Suggested actions 1 Time too sh...

Page 101: ...ellow status indicator at the front of the detector is switched ON This section describes the meaning of detector not ready messages Purge Time Running Event ID 2600 Wait for Purge Event ID 2692 Probable cause Suggested actions 1 The purge valve is open liquid is flowing through both sample and reference cell Allow the reference purge time to elapse Probable cause Suggested actions 1 The detector ...

Page 102: ...falling on the two light receiving diodes Flush the reference cell with the mobile phase being used Perform the RID Optical Balance procedure see The Optical Balance Procedure on page 115 Probable cause Suggested actions 1 There is insufficient light falling on the light receiving diodes to generate a refractive index signal Flush the flow cell with the mobile phase being used to ensure that it is...

Page 103: ...nce Procedure 115 Using the Build in Test Chromatogram 117 Procedure Using the Agilent LabAdvisor 117 ASTM Drift and Noise Test 119 Setting the Test Conditions 119 Evaluation 122 D A Converter DAC Test 123 Test Evaluation 124 Other Lab Advisor Functions 125 EMFs Early Maintenance Feature 125 This chapter describes the detector s built in test functions ...

Page 104: ...t functions Interface Comment Available Function Agilent Lab Advisor For functions see Table 9 on page 105 Available functions depend on Product Level Basic Advanced FSE Agilent ChemStation No tests available Adding of temperature lamp signals to chromatographic sig nals possible Diagnostic Signals Temperature optical unit Diode 1 2 Balance Polarity Agilent Instant Pilot G4208A No tests available ...

Page 105: ... Basic Advanced Module Info Basic Advanced Test Chromatogram Basic Advanced RID Tool Screen Basic Advanced Controls Advanced Method Parameters Attenuation Analog Output Advanced Analog Output 1 Offset Full Scale Advanced Polarity Advanced Configuration Remote Pulse Duration s Basic Advanced Analog Output 1 Range Advanced Control Recycle Basic Advanced Heater On Off Basic Advanced Method Parameters...

Page 106: ...r Reset Basic Advanced Clear Error Basic Advanced Signals RI Signal nRIU Advanced Optical Temperature C Advanced Board Temperature C Advanced Signal Diode 1 counts Advanced Signal Diode 2 counts Advanced Diode Balance Advanced Polarity Advanced EMF Counters Time since last Purge Basic Advanced Table 9 Function Overview Lab Advisor Basic Advanced Functions Product Level ...

Page 107: ...Agilent InfinityLab LC Series RID User Manual 107 8 Test Functions Introduction Figure 19 The Lab Advisor shows the available tests ...

Page 108: ...e cells have been purged with LC grade water the sucrose solution is introduced into the flow cell and then the built in refractive index calibration functionality is used Filling the sample cell with the sucrose calibration solution will give a theoretical detector response of 512 000 nRIU 5 000 nRIU The calibration algorithm will allow the actual detector response if different to be changed to t...

Page 109: ... d Dilute the contents of the flask to volume with LC grade water Wait five minutes and shake again The solution is now ready for use 2 Preparing the pump a Fill a suitable solvent bottle with LC grade water b Connect this bottle to Channel A of the pump A1 if a binary pump 3 Flush the degasser and pump When Recommended after exchange of the optical unit or RIM board Tools required Description Lab...

Page 110: ...ilent pump is part of the system the pump section is active 5 Purging the sample and reference cells a The purge valve will automatically switch to the ON position b Using a syringe or LC pump flush the sample and reference cell with about 20 mL of LC grade water If an Agilent pump is part of the system the pump section is active c The purge valve will automatically switch to the OFF position when...

Page 111: ...tal position e Remove the needle f Add the filter to the syringe and fit the needle to filter Figure 20 Syringe with Sample Filter g Lift the needle tip and carefully eject approximately 0 5 mL to remove air out of the syringe and to flush the needle h Add the PEEK fitting to the needle tip and fix both at the flow cell inlet i Slowly inject about 1 0 ml and wait for about 10 s to inject another 0...

Page 112: ...libration Performing the Calibration 1 Run the RID Calibration Screen with the Agilent Lab Advisor for further information see Online Help of user interface 2 If the purge of the sample and reference side has been done start the calibration process with OK 3 Inject the calibration sample ...

Page 113: ... nRIU enter the theoretical value 512000 in the dialog box If the detector response is within the theoretical response click OK 5 The calibration was successful NOTE Rinse the sample cell with pure water at a minimum of 1 5 mL min to flush the sucrose from the cell and the capillaries When organic solvent is sequentially applied without rinsing a blockage of capillaries may occur ...

Page 114: ...re diode1 signal proportional to the amount of light falling on diode1 diode2 signal proportional to the amount of light falling on diode2 Optical balance adjustment is a manual procedure where the position of the light beam falling on the light receiving diode is adjusted using the zero glass adjustment screw NOTE The detector will become not ready when the diode balance value falls outside the r...

Page 115: ...Switch the purge valve to the ON position b Purge the sample and reference cells for around 10 min with the solvents to be used c Switch the purge valve to the OFF position 3 Select Optical Balance When When light falling on light receiving diodes is out of balance Tools required Description Flat head screwdriver NOTE This procedure should only be performed to correct a permanent misalignment of t...

Page 116: ...ical Balance a While monitoring the optical balance use the flat headed screwdriver to turn the zero glass adjustment screw slowly b When the diode balance value reaches 0 00 green area optical balance is restored Figure 21 Turning the zero glass adjustment screw Zero glass adjustment screw left ...

Page 117: ...d either by means of a stop time or manually Procedure Using the Agilent LabAdvisor This procedure works for all Agilent 1200 Infinity detectors DAD MWD VWD FLD and RID The example figure is from the RID detector 1 Assure that the default LC method is loaded via the control software 2 Start the Agilent Lab Advisor software B 01 03 SP4 or later and open the detector s Tools selection 3 Open the tes...

Page 118: ...uild in Test Chromatogram 6 To start a test chromatogram enter in the command line STRT Figure 22 Test Chromatogram with Agilent Lab Advisor 7 To stop the test chromatogram enter in the command line STOP NOTE The test chromatogram is switched off automatically at the end of a run ...

Page 119: ...the detector 3 Set up the instrument with the following test conditions When If you want to checkout the detector Tools required Description LC system with G7162A RID Parts required p n Description 1 G1362 87301 Restriction capillary Table 10 Chromatographic Conditions Mobile phases LC grade water Column Restriction capillary 2 7 m x 1 7 mm i d Flow rate 1 0 mL min Compressibility 46 Stroke 20 µL ...

Page 120: ...abilize 7 Run the ASTM Drift and Noise Test Screen with the Agilent Lab Advisor for further information see Online Help of user interface NOTE The optical unit temperature must be set at least 5 C above ambient conditions Therefore if ambient temperature is above 30 C higher values for optical unit temperature and column compartment temperature must be set NOTE For optimum performance a stabilizat...

Page 121: ...Agilent InfinityLab LC Series RID User Manual 121 8 Test Functions ASTM Drift and Noise Test 8 Click OK The measurement starts The test has completed and shows either PASSED of FAILED ...

Page 122: ...fractive Index Detectors used in Liquid Chromatography using 0 5 minute segments Wander The long term noise in nRIU based on ASTM method E 1303 95 Practice for Refractive Index Detectors used in Liquid Chromatography using 0 5 minute segments Drift The drift in nRIU hour based on ASTM method E 1303 95 Practice for Refractive Index Detectors used in Liquid Chromatography measured over 20 minutes Fa...

Page 123: ...log signal of approximately 50 mV if the zero offset of the analog output is set to the default value of 5 which can be plotted on an integrator A continuous square wave with an amplitude of 10 µV and a frequency of approximately 1 cycle 24 seconds is applied to the signal The amplitude of the square wave and the peak to peak noise are used to evaluate the DAC test 1 Run the D A Converter DAC Test...

Page 124: ...AC Test Test Evaluation The noise on the step should be less than 3 µV Probable cause Suggested actions 1 Bad cable or grounding problem between detector and external device Check or replace the cable 2 Defective detector main board Please contact your Agilent service representa tive ...

Page 125: ...al 125 8 Test Functions Other Lab Advisor Functions Other Lab Advisor Functions EMFs Early Maintenance Feature The EMFs screen allows you to view and manage the EMF counters for all modules in all systems Figure 23 EMFs Early Maintenance Feature ...

Page 126: ...d Cautions 128 Overview of Maintenance 130 Cleaning the Module 131 Storage of the Detector 131 Remove and Install Doors 132 Flow Cell Flushing 134 Correct Leaks 135 Replace Leak Handling System Parts 138 Replace the Module Firmware 140 This chapter provides general information on maintenance and repair of the detector ...

Page 127: ...tenance and Repair Introduction to Maintenance Introduction to Maintenance The module is designed for easy maintenance Maintenance can be done from the front with module in place in the system NOTE There are no serviceable parts inside Do not open the module ...

Page 128: ...ken off when line power is still connected Never plug the power line back in when cover is removed WARNING Sharp metal edges Sharp edged parts of the equipment may cause injuries To prevent personal injury be careful when getting in contact with sharp metal areas WARNING Toxic flammable and hazardous solvents samples and reagents The handling of solvents samples and reagents can hold health and sa...

Page 129: ... 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 CAUTION Safety standards for external equipment If you connect external equipment to the instrument make sure that you only use accessory units tested and approved according to the safety standards appropriate for...

Page 130: ...e described that can be carried out without opening the main cover Table 11 Maintenance Procedures Procedure Typical Frequency Notes Flow cell flushing If flow cell is contaminated Leak sensor drying If leak has occurred Check for leaks Leak handling System replace ment If broken or corroded Check for leaks Replacing the detector s Firm ware If not up to date or corrupted ...

Page 131: ...er and mild detergent Storage of the Detector WARNING Liquid dripping into the electronic compartment of your module can cause shock hazard and damage the module Do not use an excessively damp cloth during cleaning Drain all solvent lines before opening any connections in the flow path NOTE In case the detector is not used for some time stored then fill the flow cell sample and reference side with...

Page 132: ...all Doors Parts required p n Description 5067 5745 Door Assembly Infinity 180 Left 5067 5746 Door Assembly Infinity 180 Right NOTE The figures in this procedure show the Infinity II Multisampler module as an example The principle of how to remove and or install doors works in the same way for all Infinity II modules ...

Page 133: ...ntenance and Repair Remove and Install Doors 1 Press the release buttons and pull the front door out 2 For the Installation of the front door Insert the hinges into their guides and move the door in until the release buttons click into their final position ...

Page 134: ...e WARNING Dangerous solvents The strong solvents used in this procedure are toxic and flammable and proper precautions are necessary Wear protective gloves and goggles Don t expose yourself to the vapors NOTE Aqueous solvents can build up algae and therefore should do not be left in the flow cell for long periods Add a small percentage of organic solvents e g acetonitrile or methanol 5 NOTE The st...

Page 135: ...as occurred in the valve area or at the capillary connections Tools required Description Tissue Wrench 1 4 inch for capillary connections 1 Open the doors 2 Observe the leak sensor area for leaks and correct if required 3 Observe the interface ports for leaks and correct if required 4 Unscrew the screws of the Service Door ...

Page 136: ...l 136 9 Maintenance and Repair Correct Leaks 5 Open the Service Door 6 Remove the Service Door 7 Observe the valve area for leaks and correct if required 8 Install the Service Door 9 Close the Service Door 10 Fasten the screws of the Service Door ...

Page 137: ...Agilent InfinityLab LC Series RID User Manual 137 9 Maintenance and Repair Correct Leaks 11 Close the doors ...

Page 138: ...Parts Parts required p n Description 5043 0856 Leak Adapter 5063 6527 Tubing Silicon Rubber 1 2 m ID OD 6 9 mm approximately 85 mm required 1 Open the doors 2 Locate the Leak Adapter 1 and Tubing 2 3 Press the Leak Adapter down and remove it together with the tubing 4 Install the Leak Adapter by pressing it into the Main Cover 1 2 1 2 1 2 ...

Page 139: ...ab LC Series RID User Manual 139 9 Maintenance and Repair Replace Leak Handling System Parts 5 Insert the Tubing approximately 115 mm required for replacement between Leak Adapter outlet and Leak Panel 6 Close the doors ...

Page 140: ...der versions or to keep all systems on the same validated revision The installation of older firmware might be necessary to keep all systems on the same validated revision or if a new module with newer firmware is added to a system or if third party control software requires a special version Tools required Description Agilent Lab Advisor software Parts required Description 1 Firmware tools and do...

Page 141: ...ent InfinityLab LC Series RID User Manual 141 10 Parts for Maintenance Overview of Maintenance Parts 142 Accessory Kit 144 Leak Handling Parts 147 This chapter provides information on parts for maintenance ...

Page 142: ...escription 1 5067 5745 Door Assembly Infinity 180 Left 2 5067 5746 Door Assembly Infinity 180 Right 3 5043 0856 Leak Adapter 4 5063 6527 Tubing Silicon Rubber 1 2 m ID OD 6 9 mm for Waste and Leak Adapter ca 85 mm required 5 5043 1013 Tubing Clip G1362 68706 Interface tubing kit G1362 87300 Interfacing capillary G1362 87301 Restriction capillary G7162 87300 Waste Tube Kit recycle waste ...

Page 143: ...Agilent InfinityLab LC Series RID User Manual 143 10 Parts for Maintenance Overview of Maintenance Parts Figure 24 Maintenance Parts 1 2 3 4 5 5 ...

Page 144: ...Agilent InfinityLab LC Series RID User Manual 144 10 Parts for Maintenance Accessory Kit Accessory Kit Figure 25 Accessory Kit ...

Page 145: ...Restriction capillary 3 2 0100 1700 FERRULE AY 18IN 4 2 0100 1708 Nut 1 8 PPS 5 1 G7162 87300 Waste Tube Kit recycle waste includes Fitting PK 2x Tubing 2 m 2x 1 5042 6449 Flex Tube OD 1 6 mm 1 0100 1516 Fitting PK 1 16 x 10 32 SH male nut 2 pk 6 1 0890 1760 Tubing Flexible 1 ea 1 meter 1 5181 1519 CAN cable Agilent module to module 1 m 8 2 5043 1013 Tubing Clip 9 1 5500 1155 Tube Connector 90 deg...

Page 146: ...mm x 340 mm Column to RID 2 1 G1362 87301 Restriction capillary 3 2 0100 1700 FERRULE AY 18IN 4 2 0100 1708 Nut 1 8 PPS 5 1 G7162 87300 Waste Tube Kit recycle waste includes Fitting PK 2x Tubing 2 m 2x 1 5042 6449 Flex Tube OD 1 6 mm 1 0100 1516 Fitting PK 1 16 x 10 32 SH male nut 2 pk 6 1 0890 1760 Tubing Flexible 1 ea 1 meter 1 5181 1519 CAN cable Agilent module to module 1 m 8 2 5043 1013 Tubin...

Page 147: ...tem p n Description 1 5043 0856 Leak Adapter 2 5063 6527 Tubing Silicon Rubber 1 2 m ID OD 6 9 mm 3 5061 3356 Leak Sensor Assembly 4 G7162 44111 Leak Plane 5 0515 2529 Screw Tapping PAN HD TORX T10 3x8 ST ZN 5043 1013 Tubing Clip not shown 6 G1362 44110 Leak Pan 7 0535 0030 Nut M 14 8 3050 0900 Washer 1 2 3 4 5 6 7 8 ...

Page 148: ...Manual 148 11 Identifying Cables Cable Overview 149 Analog Cables 151 Remote Cables 153 CAN LAN Cables 157 Agilent Module to PC 158 USB Cables 159 This chapter provides information on cables used with the Agilent 1200 Infinity Series modules ...

Page 149: ...ion 35900 60750 Agilent 35900A A D converter 01046 60105 Analog cable BNC to general purpose spade lugs p n Description 5188 8029 ERI to general purpose 5188 8044 Remote Cable ERI ERI 5188 8045 Remote Cable APG ERI 5188 8059 ERI Extension Cable 1 2 m 5061 3378 Remote Cable to 35900 A D converter 01046 60201 Agilent module to general purpose 5188 8057 Fraction Collection ERI remote Y cable p n Desc...

Page 150: ...d 7 m for point to point connec tion p n Description RS232 61601 RS 232 cable 2 5 m Instrument to PC 9 to 9 pin female This cable has special pin out and is not compatible with connecting printers and plotters It is also called Null Modem Cable with full handshaking where the wiring is made between pins 1 1 2 3 3 2 4 6 5 5 6 4 7 8 8 7 9 9 5181 1561 RS 232 cable 8 m p n Description 5188 8050 USB A ...

Page 151: ...s One end of these cables provides a BNC connector to be connected to Agilent modules The other end depends on the instrument to which connection is being made Agilent Module to 35900 A D converters p n 35900 60750 35900 Pin Agilent module Signal Name 1 Not connected 2 Shield Analog 3 Center Analog ...

Page 152: ...s Analog Cables Agilent Module to BNC Connector Agilent Module to General Purpose p n 8120 1840 Pin BNC Pin Agilent module Signal Name Shield Shield Analog Center Center Analog p n 01046 60105 Pin Pin Agilent module Signal Name 1 Not connected 2 Black Analog 3 Red Analog ...

Page 153: ...able 1 2 m D Sub15 pin male female p n 5188 8029 pin Color code Enhanced Remote Classic Remote Active TTL 1 white IO1 START REQUEST Low 2 brown IO2 STOP Low 3 green IO3 READY High 4 yellow IO4 POWER ON High 5 grey IO5 NOT USED 6 pink IO6 SHUT DOWN Low 7 blue IO7 START Low 8 red IO8 PREPARE Low 9 black 1wire DATA 10 violet DGND 11 grey pink 5V ERI out 12 red blue PGND 13 white green PGND 14 brown g...

Page 154: ...45 ERI to APG Connector D_Subminiature 15 pin ERI Connector D_Subminiature 9 pin APG p n 5188 8045 Pin ERI Signal Pin APG Active TTL 10 GND 1 1 Start Request 9 Low 2 Stop 8 Low 3 Ready 7 High 5 Power on 6 High 4 Future 5 6 Shut Down 4 Low 7 Start 3 Low 8 Prepare 2 Low Ground Cable Shielding NC ...

Page 155: ...a Agilent Technologies APG Analytical Products Group remote connector to be connected to Agilent modules The other end depends on the instrument to be connected to Table 12 5188 8057 ERI to APG and RJ45 p n 5188 8057 Pin ERI Signal Pin APG Active TTL Pin RJ45 10 GND 1 5 1 Start Request 9 High 2 Stop 8 High 3 Ready 7 High 4 Fraction Trig ger 5 High 4 5 Power on 6 High 6 Shut Down 4 High 7 Start 3 H...

Page 156: ... 2 Brown Prepare run Low 3 Gray 3 Gray Start Low 4 Blue 4 Blue Shut down Low 5 Pink 5 Pink Not connected 6 Yellow 6 Yellow Power on High 7 Red 7 Red Ready High 8 Green 8 Green Stop Low 9 Black 9 Black Start request Low p n 01046 60201 Wire Color Pin Agilent module Signal Name Active TTL White 1 Digital ground Brown 2 Prepare run Low Gray 3 Start Low Blue 4 Shut down Low Pink 5 Not connected Yellow...

Page 157: ...nected to Agilent modules CAN or LAN connectors CAN Cables LAN Cables p n Description 5181 1516 CAN cable Agilent module to module 0 5 m 5181 1519 CAN cable Agilent module to module 1 m p n Description 5023 0203 Cross over network cable shielded 3 m for point to point connection 5023 0202 Twisted pair network cable shielded 7 m for point to point connec tion ...

Page 158: ...cription RS232 61601 RS 232 cable 2 5 m Instrument to PC 9 to 9 pin female This cable has special pin out and is not compatible with connecting printers and plotters It is also called Null Modem Cable with full handshaking where the wiring is made between pins 1 1 2 3 3 2 4 6 5 5 6 4 7 8 8 7 9 9 5181 1561 RS 232 cable 8 m ...

Page 159: ...al 159 11 Identifying Cables USB Cables USB Cables To connect a USB Flash Drive use a USB OTG cable with Mini B plug and A socket p n Description 5188 8050 USB A M USB Mini B 3 m PC Module 5188 8049 USB A F USB Mini B M OTG Module to Flash Drive ...

Page 160: ... Rear View of the Module 166 Information on Instrument Serial Number 167 Interfaces 168 Overview Interfaces 170 ERI Enhanced Remote Interface 173 USB Universal Serial Bus 175 Setting the 6 bit Configuration Switch 176 Special Settings 178 Instrument Layout 180 Early Maintenance Feedback 181 This chapter describes the module in more detail on hardware and electronics ...

Page 161: ...phic Output The data flow is shown below Figure 26 Data flow for chromatographic output Peak width nRIU calculation A D electronics diode difference signal Diode 1 signal Diode 2 signal Selected signals Raw data Analog outputs Digital interface Analog interface Pre Filter Filter calculation zero Polarity Temperature signal Scale offset ...

Page 162: ...ies are the complete communication capabilities CAN LAN USB and RS 232 memory management ability to update the firmware of the main system Main System Its properties are the complete communication capabilities CAN LAN USB and RS 232 memory management ability to update the firmware of the resident system In addition the main system comprises the instrument functions that are divided into common fun...

Page 163: ...for example 1315B for the G1315B DAD R the firmware revision for example A for G1315B or B for the G1315C DAD VVV is the revision number for example 650 is revision 6 50 XXX is the build number of the firmware For instructions on firmware updates refer to section Replacing Firmware in chapter Maintenance or use the documentation provided with the Firmware Update Tools Figure 27 Firmware Update Mec...

Page 164: ...tial firmware revision For example a G1315C DAD SL cannot be downgraded below firmware revision B 01 02 or to a A xx xx Some modules can be re branded e g G1314C to G1314B to allow operation in specific control software environments In this case the feature set of the target type is used and the feature set of the original one is lost After re branding e g from G1314B to G1314C the original featur...

Page 165: ...ector may be used to control the module from a computer through a LAN connection This connector is activated and can be configured with the configuration switch With the appropriate software the USB connector may be used to control the module from a computer through a USB connection The power input socket accepts a line voltage of 100 240 VAC 10 with a line frequency of 50 or 60 Hz Maximum power c...

Page 166: ...Series RID User Manual 166 12 Hardware Information Electrical Connections Rear View of the Module Figure 28 Rear view of the Refractive Index Detector Configuration switch Analog output USB Mini Port LAN ERI CAN Power socket ...

Page 167: ... information on the instrument labels provide the following information CCYWWSSSSS Format CC country of manufacturing DE Germany JP Japan CN China YWW year and week of last major manufacturing change e g 820 could be week 20 of 1998 or 2008 SSSSS real serial number CCXZZ00000 Format CC Country of manufacturing DE Germany JP Japan CN China X Alphabetic character A Z used by manufacturing ZZ Alpha n...

Page 168: ...2 Analog APG A ERI E Special Pumps G7104A C 2 No Yes Yes 1 A G7110B 2 Yes Yes No No E G7111A B G5654A 2 Yes Yes No No E G7112B 2 Yes Yes No No E G7120A 2 No Yes Yes 1 A G7161A B 2 Yes Yes No No E Samplers G7129A B C 2 Yes Yes No No E G7167B C G5667A 2 Yes Yes No No E G7157A 2 Yes Yes No No E Detectors G7114A B 2 Yes Yes No 1 E G7115A 2 Yes Yes No 1 E G7117A B C 2 Yes Yes No 1 E G7121A B 2 Yes Yes ...

Page 169: ...No No No No Requires a host module with on board LAN with minimum FW B 06 40 or C 06 40 or with addi tional G1369C LAN Card G1364E F G5664B 2 Yes Yes No No E THERMOSTAT for G1330B Others G7116A B 2 No No No No No Requires a HOST mod ule via CAN G7122A No No No Yes No A G7170B 2 No No No No No Requires a host module with on board LAN with minimum FW B 06 40 or C 06 40 or with addi tional G1369C LAN...

Page 170: ...oard LAN nor an interface slot for a LAN card e g G1170A Valve Drive or G4227A Flexible Cube These are hosted modules and require a Host module with firmware B 06 40 or later or with additional G1369C LAN Card USB The USB interface replaces the RS 232 Serial interface in new FUSION generation modules For details on USB refer to USB Universal Serial Bus on page 175 Analog Signal Output The analog s...

Page 171: ...ystem s critical parts in case any module detects a serious problem To detect whether all participating modules are switched on or properly powered one line is defined to summarize the POWER ON state of all connected modules Control of analysis is maintained by signal readiness READY for next analysis followed by START of run and optional STOP of run triggered on the respective lines In addition P...

Page 172: ... Receiver is any module performing run time controlled activities 3 READY H System is ready for next analysis Receiver is any sequence con troller 4 POWER ON H All modules connected to system are switched on Receiver is any module relying on operation of others 5 Not used 6 SHUT DOWN L System has serious problem for example leak stops pump Receiver is any module capable to reduce safety risk 7 STA...

Page 173: ...nics use ERI This interface is already used in the Agilent Universal Interface Box 2 UIB2 ERI Description The ERI interface contains eight individual programmable input output pins In addition it provides 24 V power and 5 V power and a serial data line to detect and recognize further add ons that could be connected to this interface This way the interface can support various additional devices lik...

Page 174: ... Wire Data Future Use This serial line can be used to read out an EPROM or write into an EPROM of a connected ERI device The firmware can detect the connected type of device automatically and update information in the device if required Pin Enhanced Remote 1 IO 1 START REQUEST 2 IO 2 STOP 3 IO 3 READY 4 IO 4 POWER ON 5 IO 5 NOT USED 6 IO 6 SHUT DOWN 7 IO 7 START 8 IO 8 PREPARE 9 1 wire DATA 10 DGN...

Page 175: ...ble by firmware command defined turn on off For devices that need higher power Class 0 0 5 A maximum 12 W Class 1 1 0 A maximum 24 W Class 2 2 0 A maximum 48 W Class depends on hosting module s internal power overhead If a connected device requires more power the firmware detects this overcurrent detection and provides the information to the user interface Fuse used for safety protection on board ...

Page 176: ... Switch settings provide configuration parameters for LAN and instrument specific initialization procedures All modules with FUSION electronics Default is ALL switches DOWN best settings Default IP address for LAN 192 168 254 11 For specific LAN modes switches 4 5 must be set as required For boot resident cold start modes switches 1 2 or 6 must be UP Figure 30 Location of Configuration switch exam...

Page 177: ...ttings are taken from non volatile memory 0 n a 2 2 not assigned Always keep these switches on position 0 off n a LAN Init Mode n a Use Default IP Address3 3 Default IP Address is 192 168 254 11 0 0 0 0 0 Use Stored IP Address 0 0 0 1 0 Use DHCP to request IP Address4 4 Host Name will be the MAC address 0 0 1 0 0 Test 1 System n a n a n a ColdStart Boot Main System Keep Data 0 0 0 0 0 Boot Residen...

Page 178: ...t can be used to bring the module into a defined mode with default parameter settings Boot Main System Revert to Default Data The instrument will boot to main mode and changes to the module s default parameter May be also required to load resident firmware into the module Boot Resident System Revert to Default Data The instrument will boot to resident mode and changes to the module s default param...

Page 179: ...Switch Table 16 Boot Resident Forced Coldstart SW1 SW2 SW3 SW4 SW5 SW6 Init Mode 1 0 0 0 0 0 Boot Main System Keep Data 1 1 0 0 0 0 Boot Resident System Keep Data 1 0 0 0 0 1 Boot Main System Revert to Default Data 1 1 0 0 0 1 Boot Resident System Revert to Default Data Note The setting 0 down is essential ...

Page 180: ... is then housed in a metal inner cabinet which is enclosed by a plastic external cabinet The advantages of this packaging technology are virtual elimination of fixing screws bolts or ties reducing the number of components and increasing the speed of assembly disassembly the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations the pla...

Page 181: ...nterface when the limit is exceeded Some counters can be reset to zero after the required maintenance procedure Using the EMF Counters The user settable EMF limits for the EMF Counters enable the early maintenance feedback to be adapted to specific user requirements The useful maintenance cycle is dependent on the requirements for use Therefore the definition of the maximum limits need to be deter...

Page 182: ...185 Initialization Mode Selection 186 Dynamic Host Configuration Protocol DHCP 188 General Information DHCP 188 Setup DHCP 189 Manual Configuration 191 With Telnet 192 PC and Agilent ChemStation Setup 195 PC Setup for Local Configuration 195 Agilent ChemStation Setup 198 This chapter provides information on connecting the module to the Agilent ChemStation PC ...

Page 183: ...be found on a label at the rear of the module underneath the configuration switch see Figure 32 on page 183 Figure 31 MAC Label 2 Connect the instrument s LAN interface see Figure 32 on page 183 to the PC network card using a crossover network cable point to point or a hub or switch using a standard LAN cable Figure 32 Location of LAN interfaces and MAC label NOTE This chapter is generic and may s...

Page 184: ...d DHCP Server using the so called Dynamic Host Configuration Protocol This mode requires a LAN onboard Module or a G1369C LAN Interface card see Setup DHCP on page 189 by manually setting the parameters using Telnet by manually setting the parameters using the Local Controller The LAN interface differentiates between several initialization modes The initialization mode short form init mode defines...

Page 185: ...on Switches The configuration switch can be accessed at the rear of the module Figure 33 Location of Configuration switch example shows a G7114A B VWD The module is shipped with all switches set to OFF as shown above Configuration switch NOTE To perform any LAN configuration SW1 and SW2 must be set to OFF ...

Page 186: ... Using Stored is selected the parameters are taken from the non volatile memory of the module The TCP IP connection will be established using these parameters The parameters were configured previously by one of the described methods Figure 34 Using Stored Principle Table 17 Initialization Mode Switches SW1 SW2 SW3 SW4 SW5 SW6 Init Mode 0 0 0 0 0 0 Use Default IP Address 0 0 0 0 1 0 Use Stored IP A...

Page 187: ... then close the session select the initialization mode Using Stored power on again and establish the TCP IP connection using the new parameters When the module is wired to the PC directly e g using a cross over cable or a local hub separated from the local area network the user may simply keep the default parameters to establish the TCP IP connection Active Parameter Default Parameter NOTE Using t...

Page 188: ...obtained become the active parameters immediately They are not stored to the non volatile memory of the card Besides requesting the network parameters the card also submits its hostname to the DHCP Server The hostname equals the MAC address of the card e g 0030d3177321 It is the DHCP server s responsibility to forward the hostname address information to the Domain Name Server The card does not off...

Page 189: ... is on a label on the card or at the rear of the main board e g 0030d3177321 On the Local Controller the MAC address can be found under Details in the LAN section Figure 37 LAN Setting on Instant Pilot The DHCP functionality is available on all Agilent HPLC modules with on board LAN Interface or LAN Interface Card G1369C and B firmware B 06 40 or above or modules with D firmware All mod ules shoul...

Page 190: ...enLAB CDS ChemStation Edition Lab Advisor Firmware Update Tool and use MAC address as host name e g 0030d3177321 The LC system should become visible in the control software see Note in section General Information DHCP on page 188 Table 19 G1369C LAN Interface Card configuration switch on the card SW 4 SW 5 SW 6 SW 7 SW 8 Initialization Mode ON OFF OFF OFF OFF DHCP Table 20 LC Modules with 8 bit co...

Page 191: ...atile memory of the module It never affects the currently active parameters Therefore manual configuration can be done at any time A power cycle is mandatory to make the stored parameters become the active parameters given that the initialization mode selection switches are allowing it Figure 38 Manual Configuration Principle TELNET Session Control Module Stored Parameter Non Volatile RAM ...

Page 192: ...g on Windows START button and select Run Type cmd and press OK 2 Type the following at the system DOS prompt c telnet IP address or c telnet host name Figure 39 Telnet Starting a session where IP address may be the assigned address from a Bootp cycle a configuration session with the Handheld Controller or the default IP address see Configuration Switches on page 185 When the connection was establi...

Page 193: ...press Enter where parameter refers to the configuration parameter you are defining and value refers to the definitions you are assigning to that parameter Each parameter entry is followed by a carriage return Table 21 Telnet Commands Value Description displays syntax and descriptions of commands displays current LAN settings ip x x x x sets new ip address sm x x x x sets new subnet mask gw x x x x...

Page 194: ...t the LAN interface MAC address initialization mode Initialization mode is Using Stored active TCP IP settings TCP IP status here ready connected to PC with controller software e g Agilent ChemStation here not connected Figure 43 Telnet Change IP settings change of IP setting to Initialization mode is Using Stored active TCP IP settings stored TCP IP settings in non volatile memory connected to PC...

Page 195: ...t ChemStation Setup PC Setup for Local Configuration This procedure describes the change of the TCP IP settings on your PC to match the module s default parameters in a local configuration see Table 18 on page 187 1 Open the Local Area Connection Properties and select Internet Protocol TCP IP Then click on Properties ...

Page 196: ...Agilent InfinityLab LC Series RID User Manual 196 13 LAN Configuration PC and Agilent ChemStation Setup 2 You may enter here the fixed IP address of the module or use the Alternative Configuration ...

Page 197: ...Lab LC Series RID User Manual 197 13 LAN Configuration PC and Agilent ChemStation Setup 3 We will use the direct LAN access via Cross over LAN cable with the module s IP address 4 Click on OK to save the configuration ...

Page 198: ... for the 1290 Infinity system using the 1290 Infinity DAD G4212A as the interfacing module The setup works in the same way for all other systems 1 Open the ChemStation Configuration Editor 2 Select from the menu Configure Instruments 3 Select Modular 3D LC System 4 Give the Instrument a name NOTE The LAN must be connected to detector due to high data load on communication to Control Software ...

Page 199: ...LC Series RID User Manual 199 13 LAN Configuration PC and Agilent ChemStation Setup 5 Click on OK 6 Select LC System Access Access Point and click on Add 7 Click on OK The Configuration Editor shows now the new instrument ...

Page 200: ...ons 9 Save the current configuration via File Save 10 Exit the Configuration Editor 11 Start the Agilent ChemStation During first startup or when the system configuration has changed a notification shows up 12 The left column shows the modules that could be configured You may select the module manually from the list We use the Auto Configuration mode Click on Yes ...

Page 201: ...Setup 13 Enter the IP address or the Hostname of the module with the LAN access 14 Click on OK The selected module is shown now in the right window with serial number In addition all other modules connected via CAN to the detector are shown as well 15 Click on OK to continue the ChemStation loading ...

Page 202: ...LAN Configuration PC and Agilent ChemStation Setup 16 You may see the details of the module by selecting the module and clicking on Configure Under Connection Settings you may change the IP Hostname of the module may require a re start of the ChemStation ...

Page 203: ... Manual 203 13 LAN Configuration PC and Agilent ChemStation Setup After successful load of the ChemStation you should see the module s as active item in the graphical user interface GUI Figure 45 Screen After Successful Load of ChemStation ...

Page 204: ...ent 206 Do Not Operate in an Explosive Atmosphere 207 Do Not Remove the Instrument Cover 207 Do Not Modify the Instrument 207 In Case of Damage 207 Solvents 208 Safety Symbols 209 Waste Electrical and Electronic Equipment WEEE Directive 211 Radio Interference 212 Sound Emission 213 Solvent Information 214 Agilent Technologies on Internet 216 This chapter provides safetey and other general informat...

Page 205: ...es 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 General Do not use this product in any manner not specified by the manufacturer The protective features of this product may be impaired if it ...

Page 206: ...nce with safety or EMC regulations Make all connections to the unit before applying power NOTE Note the instrument s external markings described under Safety Symbols on page 209 WARNING Missing electrical ground Electrical shock If your product is provided with a grounding type power plug the instrument chassis and cover must be connected to an electrical ground to minimize shock hazard The ground...

Page 207: ...sence of flammable gases or fumes Explosion hazard Do not operate the instrument in the presence of flammable gases or fumes WARNING Instrument covers removed Electrical shock Do Not Remove the Instrument Cover Only Agilent authorized personnel are allowed to remove instrument covers Always disconnect the power cables and any external circuits before removing the instrument cover WARNING Damage to...

Page 208: ...nt For the solvents methanol and ethanol keep the solvent temperature at least 25 K below the boiling point Do not operate the instrument in an explosive atmosphere Do not use solvents of ignition Class IIC according IEC 60079 20 1 for example carbon disulfide Reduce the volume of substances to the minimum required for the analysis Never exceed the maximum permissible volume of solvents 8 L in the...

Page 209: ... potential GWP see instrument label Flammable Material For Sample Thermostat which uses flammable refrigerant consult Agilent Information Center User Manual before attempting to install or service this equipment All safety precautions must be followed Confirms that a manufactured product complies with all applicable Euro pean Community directives The European Declaration of Conformity is available...

Page 210: ...evices and objects that could be damaged by strong magnetic fields Indicates a pinching or crushing hazard Indicates a piercing or cutting hazard Table 22 Symbols WARNING A WARNING alerts you to situations that could cause physical injury or death 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 c...

Page 211: ...E Directive 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 http www agilent com for more information ...

Page 212: ...ide optimized protection against radio interference All cables are in compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with unscreened cables or used for measurements on open set ups the user has to assure that under operating conditions the radio interference limits are still met within the premises ...

Page 213: ...aration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991 This product has a sound pressure emission at the operator position 70 dB Sound Pressure Lp 70 dB A At Operator Position Normal Operation According to ISO 7779 1988 EN 27779 1991 Type Test ...

Page 214: ... on the use of solvents Brown glass ware can avoid growth of algae Small particles can permanently block capillaries and valves Therefore always filter solvents through 0 4 µm filters Avoid the use of the following steel corrosive solvents solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on high concentrations of inorganic acids like sulfu...

Page 215: ...example THF dioxane diisopropyl ether should be filtered through dry aluminium oxide which adsorbs the peroxides solvents containing strong complexing agents e g EDTA mixtures of carbon tetrachloride with 2 propanol or THF Avoid the use of dimethyl formamide DMF Polyvinylidene fluoride PVDF which is used in leak sensors is not resistant to DMF ...

Page 216: ...Series RID User Manual 216 14 Appendix Agilent Technologies on Internet Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com ...

Page 217: ...ains technical reference information about the Agilent 1290 Infinity II Refractive Index Detector G7162B and the Agilent 1260 Infinity II Refractive Index Detector G7162A introduction specifications configuration optimizing troubleshooting and diagnostics maintenance parts identification hardware information safety and related information ...

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