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Agilent InfinityLab LC Series Diode Array Detectors User Manual

Optimizing the Detector

Optimizing the Detector Regarding to the System

Optimizing the Detector Regarding to the

System

Delay Volume and Extra-Column Volume

The

delay volume

is defined as the system volume between the point of mixing in

the pump and the front of the column.
The

extra-column volume

is defined as the volume between the injection point

and the detection point, excluding the volume in the column.

Extra-Column Volume

Extra-column volume is a source of peak dispersion that will reduce the

resolution of the separation and so should be minimized. Smaller diameter

columns require proportionally smaller extra-column volumes to keep peak

dispersion at a minimum.
In a liquid chromatograph the extra-column volume will depend on the

connection tubing between the autosampler, column and detector; and on the

volume of the flow cell in the detector. The extra-column volume is minimized

with the Agilent InfinityLab LC Series system due to the narrow-bore (0.12 mm

i.d.) tubing, the low-volume heat exchangers in the column compartment and the

flow cell in the detector.

How to Configure the Optimum Delay Volume

To maintain resolution in the Agilent 1290 Infinity II DAD/Agilent 1290 Infinity

DAD FS the 10 mm Max-Light cartridge cell has a low dispersion volume

(



volume 1.0 µL) and no further volume optimization is required. In situations

where the alternative 60 mm Max-Light high sensitivity cell is used to get higher

sensitivity the cell volume is optimized for the use with 3 mm and 4.6 mm inner

diameter columns.

Содержание G7117C

Страница 1: ...Diode Array Detectors Agilent InfinityLab LC Series User Manual Agilent InfinityLab LC Series Diode Array Detectors User Manual...

Страница 2: ...terial 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 furnis...

Страница 3: ...quirements and Specifications This chapter provides information on environmental requirements physical and performance specifications 3 Using the Module This chapter explains the essential operational...

Страница 4: ...apter 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 ch...

Страница 5: ...ments 26 Physical Specifications 29 Performance Specifications 30 3 Using the Module 37 Magnets 38 Turn on off 39 Status Indicators 41 Instrument Configuration 42 Set up the Detector with Agilent Open...

Страница 6: ...ts vs User Interfaces 105 Agilent Lab Advisor Software 107 7 Error Information 108 What Are Error Messages 109 General Error Messages 110 Detector Error Messages 116 8 Test Functions and Calibration 1...

Страница 7: ...e Cell 166 Correcting Leaks 167 Replace Leak Handling System Parts 168 Replace the Module Firmware 170 Information from Module s Assemblies 171 10 Parts and Materials for Maintenance 172 Overview of M...

Страница 8: ...on 207 Configuration Switches 208 Initialization Mode Selection 209 Dynamic Host Configuration Protocol DHCP 211 Manual Configuration 214 14 Appendix 219 General Safety Information 220 Waste Electrica...

Страница 9: ...uct Description G7117A 11 Product Description G7117B 12 Product Description G7117C 13 Optical System 14 Lamp 15 Max Light Cartridge Flow Cell 15 Slit Assembly 16 Grating and Diode Array 18 Leak and Wa...

Страница 10: ...page 15 More reliable and robust peak integration process automated due to less baseline noise drift refractive index and thermal effects especially under ultra fast gradient conditions RFID tracking...

Страница 11: ...spersions effects With typical detector noise levels of 0 6 AU cm the 60 mm flow cell gives up to 10 times higher sensitivity than detectors with conventional flow cells Any compromising refractive in...

Страница 12: ...ts With typical detector noise levels of 0 6 AU cm the 60 mm flow cell gives up to 10 times higher sensitivity than detectors with conventional flow cells Any compromising refractive index and thermal...

Страница 13: ...ns effects With typical detector noise levels of 0 6 AU cm the 60 mm flow cell gives up to 10 times higher sensitivity than detectors with conventional flow cells Figure 3 Overview of the detector Any...

Страница 14: ...nge Its light is focused by a lamp mirror 2 onto the entrance of the Max light cartridge flow cell 3 with optofluidic waveguides The light leaves the Max light cartridge flow cell at the other side an...

Страница 15: ...and bio inert applications are available For testing of the detector a Max Light Cartridge Test Cell is available The optical principle of the Max Light Cartridge cell is based on opto fluidic wavegui...

Страница 16: ...lities of bulk micro machining It combines the required optical functions slit and shutter in a simple and compact component The slit width is directly controlled by the micro processor of the instrum...

Страница 17: ...e of slitwidth on resolution and noise level Fixed Slit G7117A G7117C The fixed slit combines the required optical functions slit and shutter in a simple and compact component The slit width is fixed...

Страница 18: ...hed by using a concave holographic grating The grating separates the light beam into all its component wavelengths and reflects the light onto the photodiode array The diode array is a series of 1024...

Страница 19: ...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 han...

Страница 20: ...Agilent InfinityLab LC Series Diode Array Detectors User Manual 20 1 Introduction Leak and Waste Handling Figure 10 Infinity II Leak Waste Concept Flex Bench installation...

Страница 21: ...Agilent InfinityLab LC Series Diode Array Detectors User Manual 21 1 Introduction Leak and Waste Handling Figure 11 Infinity II Single Stack Leak Waste Concept bench installation...

Страница 22: ...er Manual 22 1 Introduction Leak and Waste Handling Figure 12 Infinity II Two Stack Leak Waste Concept bench installation The waste tube connected to the leak plane outlet on each of the bottom instru...

Страница 23: ...duction Leak and Waste Handling Waste Concept 1 Agilent recommends using the 6 L waste can with 1 Stay Safe cap GL45 with 4 ports 5043 1221 for optimal and safe waste disposal If you decide to use you...

Страница 24: ...Agilent InfinityLab LC Series Diode Array Detectors User Manual 24 1 Introduction Operating Principle Operating Principle Figure 13 Hydraulic path Column Waste Flow cell cartridge In Out...

Страница 25: ...2 Site Requirements and Specifications Site Requirements 26 Physical Specifications 29 Performance Specifications 30 Specifications 30 Specification Conditions 36 This chapter provides information on...

Страница 26: ...work at the module can lead to personal injuries e g shock hazard when the cover is opened and the module is connected to power Make sure that it is always possible to access the power plug Remove th...

Страница 27: ...ded purposes 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 Te...

Страница 28: ...on these 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...

Страница 29: ...396 x 436 mm 5 5 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 110 VA 100 W Ambient operating tempera ture 4 40 C 39 104 F Ambie...

Страница 30: ...hort term signal noise ASTM With 10 mm Max Light cartridge cell 3 10 6 AU at 230 nm slit width 4 nm TC 2 s With 60 mm Max Light cartridge cell 0 6 10 6 AU at 230 nm slit width 4 nm TC 2 s Drift 0 5 10...

Страница 31: ...lent Instant Pilot G4208A B 02 19 or above Communication LAN Controller Area Network CAN USB ERI ready start stop and shut down signals GLP RFID for electronics records of flow cell and UV lamp condit...

Страница 32: ...ically 2 5 AU 5 Wavelength range 190 640 nm Wavelength accuracy 1 nm self calibration with deuterium lines Wavelength precision 0 1 nm Wavelength bunching 2 400 nm programmable in 1 nm steps Slit widt...

Страница 33: ...e product number serial number test passed usage Early maintenance feedback EMF for continuous tracking of instrument usage in terms of lamp burn time with user settable limits and feedback messages E...

Страница 34: ...Wavelength range 190 640 nm Wavelength accuracy 1 nm self calibration with deuterium lines Wavelength precision 0 1 nm Wavelength bunching 2 400 nm programmable in 1 nm steps Slit width 4 nm Diode wid...

Страница 35: ...inuous tracking of instrument usage in terms of lamp burn time with user settable limits and feedback messages Electronic records of maintenance and errors Verification of wavelength accuracy with deu...

Страница 36: ...er one hour period Our published drift specification is based on these conditions Larger ambient temperature changes will result in larger drift Better drift performance depends on better control of t...

Страница 37: ...ets 38 Turn on off 39 Status Indicators 41 Instrument Configuration 42 Set up the Detector with Agilent Open Lab ChemStation 44 The Detector User Interface 45 Detector Control Settings 47 Method Param...

Страница 38: ...Agilent InfinityLab LC Series Diode Array Detectors User Manual 38 3 Using the Module Magnets Magnets 1 Magnets in doors of pumps autosamplers detectors and fraction collectors...

Страница 39: ...Agilent InfinityLab LC Series Diode Array Detectors User Manual 39 3 Using the Module Turn on off Turn on off This procedure exemplarily shows an arbitrary LC stack configuration 1 2 Power switch On...

Страница 40: ...Agilent InfinityLab LC Series Diode Array Detectors User Manual 40 3 Using the Module Turn on off 3 Turn instrument On Off with the control software 4 Power switch Off 5...

Страница 41: ...of six possible 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...

Страница 42: ...ment Configuration 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...

Страница 43: ...ay Detectors User Manual 43 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 Adv...

Страница 44: ...the Agilent OpenLab ChemStation C 01 07 and Driver A 02 14 Figure 14 ChemStation Method and Run Control just detector is shown After successful load of the OpenLab ChemStation you should see the modul...

Страница 45: ...D tag information is displayed when moving with the mouse cursor on to the tag attached to the flow cell or lamp The information provides flow cell and lamp related informa tion like Part number Produ...

Страница 46: ...e 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...

Страница 47: ...be ignited A compatible mode has to be selected based on the used lamp see Non RFID tag lamp information below Manual by PN uses the selected heat ing mode This mode can also be used when the RFID ta...

Страница 48: ...gs are available 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 addi...

Страница 49: ...The peak detector ignores any peaks that are consid erably narrower or wider than the peak width setting The response time is the time between 10 and 90 of the out put signal in response to an input s...

Страница 50: ...gnal handling to increase the margin for negative absorbance Use this option if for example your solvent gradient produces a decreasing baseline absorbance and for GPC analyses Limits 100 to 4000 mAU...

Страница 51: ...d on the chosen function a certain parameter can be selected Instrument Curves The detector has several signals internal temperatures volt ages of lamps that can be used for diagnosing problems These...

Страница 52: ...Requirements and Conditions 57 Preparing the Detector 59 Preparing the HPLC System 59 Running the Sample and Verifying the Results 61 Solvent Information 62 Capillary Coding Guide 68 Syntax for Capill...

Страница 53: ...rature at least 40 C 72 F below the boiling point of the solvent used This includes the solvent temperature in the sample compartment For the solvents methanol and ethanol keep the solvent temperature...

Страница 54: ...ng the 6 L waste can with 1 Stay Safe cap GL45 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 liq...

Страница 55: ...bout special settings Before Using the System Solvent Information Observe recommendations on the use of solvents in chapter Solvents in the pump s reference manual Priming and Purging the System When...

Страница 56: ...t 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 system when...

Страница 57: ...57 Table 7 What you will need Agilent 1200 Infinity Series system Pump plus degassing Autosampler Detector standard flow cell installed Degasser optional Column Compartment optional Agilent CDS Syste...

Страница 58: ...omatogram for this analysis is shown in Figure 18 on page 58 The exact profile of the chromatogram will depend on the chromatographic conditions Variations in solvent quality column packing standard c...

Страница 59: ...doors When the system includes a G1316 TCC typically located below the detector and its front panel is removed while the TCC is set to high temperatures the up streaming air could influence the stabil...

Страница 60: ...s Diode Array Detectors User Manual 60 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...

Страница 61: ...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 20 Chromatogram with...

Страница 62: ...cellent 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 res...

Страница 63: ...ant to dilute solutions of most inorganic acids but it can be attacked by some organic compounds and oxidizing reagents Nonoxidizing inorganic acids such as sulfuric acid and phosphoric acid have litt...

Страница 64: ...so used by Agilent Polyimide is stable in a pH range between 1 and 10 and in most organic solvents It is incompatible with concentrated mineral acids e g sulphuric acid glacial acetic acid DMSO and TH...

Страница 65: ...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 Th...

Страница 66: ...on in anhydrous 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...

Страница 67: ...polymer 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 o...

Страница 68: ...illary coding guide Type The type gives some indication on the pri mary function like a loop or a connection capillary Material The material indicates which raw material is used Fitting left fitting r...

Страница 69: ...1200 bar B Bio P PEEK I Intermedi ate 1 Fused silica in contact with solvent 2 Stainless steel coated PEEK Table 9 Capillary coding guide Type The type gives some indication on the pri mary function...

Страница 70: ...g Internal diameter in mm Color code 0 015 Orange 0 025 Yellow 0 05 Beige 0 075 Black 0 075 MP35N Black with orange stripe 0 1 Purple 0 12 Red 0 12 MP35N Red with orange stripe 0 17 Green 0 17 MP35N G...

Страница 71: ...SL long socket 5500 1250 ICC Heat Exchanger Column InfinityLab Quick Turn Capillary ST 0 17 mm x 105 mm long socket 5500 1193 MCT Heat Exchanger Column InfinityLab Quick Turn Capillary ST 0 12 mm x 2...

Страница 72: ...tions for 1260 Infinity II Bio inert LC p n From To Bottle Head Assembly G7120 60007 Solvent Bottle Infinity II Pump Capillary Ti 0 17 mm x 500 mm SL SLV 5500 1264 Pump Multisampler Capillary PK ST 0...

Страница 73: ...illary MP35N 0 17 mm x 500 mm SI SI 5500 1419 Pump Multisampler Capillary MP35N 0 12 mm x 500 mm SI SI 5500 1279 Multisampler MCT Quick Connect Capillary MP35N 0 12 mm x 105 mm 5500 1578 MCT Heat Exch...

Страница 74: ...the fit ting which forces the ferrule to seat onto the tubing or capillary NOTE Don t overtighten Overtightening will shorten the lifetime of the fitting 5 Loosen the nut and verify that the ferrule...

Страница 75: ...sion 83 Flow Cell Path Length 83 Peak width response time 85 Sample and Reference Wavelength and Bandwidth 87 Slit Width G7117B 90 Optimizing Spectral Acquisition 92 Margin for Negative Absorbance 93...

Страница 76: ...sitivity selectivity and linearity spectral sensitivity and resolution DAD only and disk space required for storing data How to Get the Best Detector Performance The information below will guide you o...

Страница 77: ...nm and 360 0 nm 100 nm as reference wavelength Set the sample wavelength to a peak or valley to get best linearity in general select a valley to get best linearity for high concentrations sensitivity...

Страница 78: ...l can be used with the G7117A DAD FS and G7117B DAD The cell is a requirement for the Ultra Low Dispersion Kit solution which currently exists as 1290 Infinity Ultra Low Dispersion Kit 5067 5189 The c...

Страница 79: ...lution Recommendations For G4212 60007 and G4212 60008 For G4212 60007 and G4212 60008 The use of Peek FS capillaries is not recommended In combination with the SST zero dead volume fitting e g at the...

Страница 80: ...standard Max Light Cartridge Cell 10 mm To install the Aperture simply screw it on the light inlet of the Max Light Cartridge Cell LSS 10 mm V 1 0 L G7117 60020 Do not apply any tools to affix the Ape...

Страница 81: ...bar On overpressure typically above 80 bar it releases the pressure to waste Application Information For the analysis and characterization of proteins and large biomolecules and applications with mob...

Страница 82: ...will measure 6 times the background absorption as in case of the 10 mm cell which will reduce the remaining dynamic absorbance range for sample peaks Furthermore those UV absorbing modifiers could com...

Страница 83: ...is the path length of the cell used for the measurement The detector can now output the signal in two forms 1 In Absorbance divide by the path length AU cm that is then similar to x C Advantage sampl...

Страница 84: ...results multiply it by the flow rate and divide it by 3 Traditionally LC analysis with UV detectors is based on comparing measurements with internal or external standards To check photometric accuracy...

Страница 85: ...ms and spectra Figure 22 Influence of Response Time on Signal and Noise Table 17 on page 86 and Table 18 on page 86 list the filter choices of the detector To get optimum results set peak width as clo...

Страница 86: ...015625 0 03125 160 160 80 40 20 0 003125 0 0625 80 80 80 40 20 0 00625 0 125 40 40 40 40 20 0 0125 0 25 20 20 20 20 20 0 025 0 5 10 10 10 10 10 0 05 1 5 5 5 5 5 0 1 2 2 5 2 5 2 5 2 5 2 5 0 2 4 1 25 1...

Страница 87: ...ls with these properties sample wavelength the center of a wavelength band with the width of sample bandwidth BW and optionally reference wavelength the center of a wavelength band with the width of r...

Страница 88: ...sample wavelength to the peak of the absorbance band that is 252 nm and the sample bandwidth to the width of the absorbance band that is 30 nm A reference of 360 100 is adequate Anisic acid does not...

Страница 89: ...length is highly recommended to further reduce baseline drift and wander induced by room temperature fluctuations or refractive index changes during a gradient An example of the reduction of baseline...

Страница 90: ...trograph This is an effective tool to adapt the detector to changing demand of different analytical problems A narrow slit provides spectral resolution for analytes with very fine structures in the ab...

Страница 91: ...lower baseline noise as shown in Figure 27 on page 91 Figure 27 Influence of the Slit Width on Baseline Noise However with a wider slit the spectrograph s optical resolution its ability to distinguis...

Страница 92: ...nearity Use a wide 8 nm slit when your sample contains very small concentrations Always use signals with bandwidth at least as wide as the slit width Optimizing Spectral Acquisition Storage of all spe...

Страница 93: ...ative Absorbance The detector adjusts its gain during balance such that the baseline may drift slightly negative about 100 mAU In some special case for example when gradient with absorbing solvents ar...

Страница 94: ...ak suppression or signal subtraction As an example the analysis of hydrochlorothiazide in the presence of caffeine is described If hydrochlorothiazide is analyzed in biological samples there is always...

Страница 95: ...n be suppressed if caffeine is to be quantified In this case the wavelength is set to 204 nm and the reference wavelength to 260 nm Figure 29 on page 95 shows the chromatographic results of the peak s...

Страница 96: ...umn volumes to keep peak dispersion at a minimum In a liquid chromatograph the extra column volume will depend on the connection tubing between the autosampler column and detector and on the volume of...

Страница 97: ...bout 2 L for this cell for example 0 02 min x 200 L min 4 L The Max Light high sensitivity cell has a path length of 60 mm and this will give between three and five times increase in signal to noise v...

Страница 98: ...row range The narrow band can be optimized for sensitivity for a specific molecule As the bandwidth is increased the signal is reduced but so is the noise and there will be an optimum for best S N As...

Страница 99: ...o reduce drift or wander in the chromatogram caused by refractive index changes due to room temperature fluctuation or gradient operation The effect of a reference signal can be easily tested by setti...

Страница 100: ...w it will increase the baseline noise unnecessarily Essentially the software uses this value to set the data collection rate such that it collects enough data points over the narrowest peaks and it is...

Страница 101: ...0 0015625 0 015625 120 120 40 20 0 0015625 0 03125 120 120 40 20 0 003125 0 0625 80 80 40 20 0 00625 0 125 40 40 40 20 0 0125 0 25 20 20 20 20 0 025 0 5 10 10 10 10 0 05 1 5 5 5 5 0 1 2 2 5 2 5 2 5 2...

Страница 102: ...of the heater functionality 1 to 30 minutes the heater control is OFF and the heater element runs at 40 duty cycle After 30 minutes the heater control is ON and is working with optimized parameters to...

Страница 103: ...Agilent InfinityLab LC Series Diode Array Detectors User Manual 103 5 Optimizing the Detector Warm up of the Detector Figure 31 Detector Warm up 1st hour Figure 32 Detector Warm up 2nd hour...

Страница 104: ...Lab LC Series Diode Array Detectors User Manual 104 6 Troubleshooting and Diagnostics Available Tests vs User Interfaces 105 Agilent Lab Advisor Software 107 Overview about the troubleshooting and dia...

Страница 105: ...Advisor Software on page 107 Screenshots used within these procedures are based on the Agilent Lab Advisor software NOTE Depending on the used interface the available tests and the screens reports may...

Страница 106: ...Agilent InfinityLab LC Series Diode Array Detectors User Manual 106 6 Troubleshooting and Diagnostics Available Tests vs User Interfaces...

Страница 107: ...d Lab Advisor Basic is 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 i...

Страница 108: ...lation 115 ERI Messages 115 Detector Error Messages 116 Diode Current Leakage 116 UV Lamp Current 116 UV Lamp Voltage 117 UV Ignition Failed 117 UV Heater Current 118 Calibration Values Invalid 118 Wa...

Страница 109: ...et a notification 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...

Страница 110: ...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...

Страница 111: ...stem configuration If one or more of the modules is no longer recognized as being connected to the system the error message is generated Probable cause Suggested actions 1 Not ready condition in one o...

Страница 112: ...n defined limits If the current falls outside the lower limit the error message is generated Probable cause Suggested actions 1 Defective leak sensor Please contact your Agilent service representa tiv...

Страница 113: ...power switch board in the module has failed open circuit The resistance across the temperature compensation sensor NTC on the power switch board is dependent on ambient temperature The change in resi...

Страница 114: ...the module The signals from the two temperature sensors leak sensor and board mounted temperature compensation sensor are used by the leak algorithm to determine whether a leak is present When a leak...

Страница 115: ...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 a...

Страница 116: ...lly monitors the anode current drawn by the lamp during operation If the anode current falls below the lower current limit the error message is generated Probable cause Suggested actions 1 Defective P...

Страница 117: ...econds the error message is generated Probable cause Suggested actions 1 Defective UV lamp or non Agilent lamp Exchange the UV lamp 2 Defective detector main board Please contact your Agilent service...

Страница 118: ...hecks if the calibration data are valid If the data are invalid or cannot be read from the spectrometer ROM the error message is generated Probable cause Suggested actions 1 Lamp disconnected Ensure t...

Страница 119: ...Error ID 1071 This temperature sensor located on the detector main board delivered a value outside the allowed range The parameter of this event equals the measured temperature in 1 100 centigrade As...

Страница 120: ...e available power of the heater reached either the upper or lower limit This event is sent only once per run The parameter determines which limit has been hit 0 means upper power limit hit excessive a...

Страница 121: ...d low ratio value 133 Quick Noise Test 134 Test Failed 136 ASTM Drift and Noise Test 137 Test Failed 139 Slit Test 140 Slit Test G7117B 140 Test Failed 141 Slit Test G7117A G7117C 142 Wavelength Verif...

Страница 122: ...verview Lab Advisor G7117A Table 22 on page 122 Available functions depend on Product Level Basic Advanced FSE Agilent ChemStation No tests available Adding of temperature lamp signals to chromatograp...

Страница 123: ...ffset Full Scale Advanced Configuration Remote Pulse Duration s Basic Advanced Analog Output 1 Range Advanced Control UV Lamp Basic Advanced Balance Detector Advanced Conversions G7117B allows G7117A...

Страница 124: ...et Basic Advanced Actuals Signal A mAU Advanced Statemachines UV Lamp Basic Advanced Signals Signal A mAU Advanced Lamp Voltage V Advanced Board Temperature C Advanced Optical Temperature C Advanced E...

Страница 125: ...Agilent InfinityLab LC Series Diode Array Detectors User Manual 125 8 Test Functions and Calibration Introduction Figure 33 The Lab Advisor shows the available test...

Страница 126: ...l differs in the low UV range then absorbing solvents are in the cell and should be flushed out See also Clean the Max Light Cartridge Cell on page 165 Below table gives an idea on the signal height v...

Страница 127: ...the temperature regulation of the optical unit is working not active during the first 30 minutes after turn on If the detector is on tests can be performed usually 10 minutes after the UV lamp has be...

Страница 128: ...urrent Test Intensity Test Wavelength Verification Test ASTM Noise Test a simplified version of the ASTM Drift and Noise Test without testing the Drift When For complete detector check Parts required...

Страница 129: ...Manual 129 8 Test Functions and Calibration Self Test 1 Run the Self Test with Agilent Lab Advisor for further information see Online Help of user interface Figure 34 Self Test Results Under the tab...

Страница 130: ...the 4 nm fixed slit is used To eliminate effects due to absorbing solvents the test should be done with water in the Max Light Cartridge Cell or with the Max Light Cartridge Test Cell The shape of th...

Страница 131: ...bble in flow cell Ensure the flow cell is filled with water and free from air bubbles Repeat test with Max Light Cartridge Test Cell and compare results 2 Incorrect calibration Recalibrate and repeat...

Страница 132: ...On the G7117A G7117C the 4 nm fixed slit is used This test should be performed initially with a new detector flow cell The values should be kept for later reference comparison 5 Old UV lamp Exchange t...

Страница 133: ...Figure 37 Cell Test Results Figure 38 Cell Test Signals example shows low intensity for flow cell Test Failed low ratio value Cell Test Evaluation Probable cause Suggested actions 1 Absorbing solvent...

Страница 134: ...minute intervals and is based on the accumulated peak to peak noise for the intervals At least seven data points per cycles are used in the calculation The cycles in the noise determination are not o...

Страница 135: ...ors User Manual 135 8 Test Functions and Calibration Quick Noise Test 1 Run the Quick Noise Test with Agilent Lab Advisor for further information see Online Help of user interface Figure 39 Quick Nois...

Страница 136: ...actions 1 Insufficient lamp warm up time Allow detector and UV lamp turned on for at least 2 hours 2 Absorbing solvent or air bubble in flow cell Ensure the flow cell is filled with water and free fr...

Страница 137: ...also part of the Self Test without checking for the drift If the test is performed with the Max Light Cartridge Test Cell the test results are not influenced by solvent or pump effects When In case o...

Страница 138: ...8 8 Test Functions and Calibration ASTM Drift and Noise Test 1 Run the ASTM Drift and Noise Test with Agilent Lab Advisor for further information see Online Help of user interface Figure 41 ASTM Drift...

Страница 139: ...warm up time Allow detector and UV lamp turned on for at least 2 hours 2 Absorbing solvent or air bubble in flow cell Ensure the flow cell is filled with water and free from air bubbles 3 Dirty or con...

Страница 140: ...p move to smaller slit or intensity increase move to larger slit must be within a defined range If the intensity changes are outside the expected range the test fails 1 Run the SlitTest with the Agile...

Страница 141: ...r bubble in Max Light Cartridge Cell Flush the flow cell or use the Max Light Cartridge Test Cell 2 Old lamp Run the Intensity Test Exchange the lamp if old or defective 3 Defective slit assembly Plea...

Страница 142: ...42 8 Test Functions and Calibration Slit Test Slit Test G7117A G7117C There is no dedicated slit test for the G7117A G7117C To verify the proper function perform the following tests Intensity Test tes...

Страница 143: ...fects When The detector is calibrated at the factory and under normal operating conditions should not require recalibration However it is advisable to recalibrate after repair of components in the opt...

Страница 144: ...rs User Manual 144 8 Test Functions and Calibration Wavelength Verification Test 1 Run the Wavelength Verification Test with the Agilent Lab Advisor for further information see Online Help of user int...

Страница 145: ...onditions should not require recalibration However it is advisable to recalibrate after maintenance flow cell or UV lamp after repair of components in the optical unit after exchange of the optical un...

Страница 146: ...on Wavelength Calibration 1 Run the Wavelength Calibration with the Agilent Lab Advisor for further information see Online Help of user interface Figure 46 Wavelength Calibration Results If you select...

Страница 147: ...ith Max Light Cartridge Test Cell and compare results 2 Dirty or contaminated Max Light Cartridge Cell Ensure the Max Light Cartridge Cell is filled with water Recalibrate 3 Old UV lamp Exchange the U...

Страница 148: ...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 V and a fr...

Страница 149: ...48 D A Converter DAC Test Example of Integrator Plot Test Evaluation The noise on the step should be less than 3 V Probable cause Suggested actions 1 Bad cable or grounding problem between detector a...

Страница 150: ...ths During the test the slit assembly moves to the dark position cutting off all light falling onto the diode array Next the leakage current from each diode is measured and displayed graphically The l...

Страница 151: ...bable cause Suggested actions 1 Defective slit assembly stray light Run the Self Test on page 128 Run the Slit Test G7117B on page 140 part of the Self Test on page 128 2 Defective detector main board...

Страница 152: ...Detectors User Manual 152 8 Test Functions and Calibration Other Lab Advisor Functions Other Lab Advisor Functions EMFs Early Maintenance Feature The EMFs screen allows you to view and manage the EMF...

Страница 153: ...e Module 157 Remove and Install Doors 157 Replace the Deuterium Lamp 159 Replace the Max Light Cartridge Cell 162 Clean the Max Light Cartridge Cell 165 Storage of Max Light Cartridge Cell 166 Correct...

Страница 154: ...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 mater...

Страница 155: ...or any damages caused in whole or in part by improper use of the products unauthorized alterations adjustments or modifications to the products failure to comply with procedures in Agilent product use...

Страница 156: ...uency Notes Cleaning of module If required Deuterium lamp exchange If noise and or drift exceeds your application limits or lamp does not ignite A wavelength calibration test and an intensity test sho...

Страница 157: ...lectronic 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 flo...

Страница 158: ...nual 158 9 Maintenance 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 i...

Страница 159: ...p does not ignite Tools required Description Screwdriver POZI 1 PT3 Parts required p n Description 1 5190 0917 Long life Deuterium lamp 8 pin with RFID tag Preparations Turn the lamp off WARNING Injur...

Страница 160: ...ottom of the cover 4 Unplug the lamp connector 1 and unscrew the two lamp screws 2 Pozidriv 5 Remove the lamp and place it on a clean place NOTE Do not touch the glass bulb with your fingers It may re...

Страница 161: ...Manual 161 9 Maintenance Replace the Deuterium Lamp 9 Slide the lamp cover into the top position of the metal front 1 and press the lamp cover completely in until it clicks 2 10 Close the doors 11 Pe...

Страница 162: ...10 mm V 1 0 L G4212 60007 Max Light Cartridge Cell 60 mm V 4 0 L G4212 60011 Max Light Cartridge Test Cell G4212 60032 HDR Max Light Cartridge Cell 3 7 mm V 0 4 L G4212 60038 ULD Max Light Cartridge...

Страница 163: ...ace the Max Light Cartridge Cell Install the Max Light Cartridge Cell 3 Flip the cartridge lever towards the front down 4 Pull the cartridge holder completely out 5 Remove the flow cell cartridge 1 In...

Страница 164: ...ay Detectors User Manual 164 9 Maintenance Replace the Max Light Cartridge Cell 3 Lift the cartridge lever up into the final position 4 Reconnect the capillaries 5 Close the doors 6 Perform a Cell Tes...

Страница 165: ...fill the flow cell with cleaning fluid The following cleaning protocols are recommended Maximum 3 hours at 25 30 C or 30 40 min at 30 35 C 6 Repeat step 4 on page 165 7 If tests fail again the flow ce...

Страница 166: ...Cell with iso propanol or methanol and insert the plugs into the cell inlet and outlet see Replace the Max Light Cartridge Cell on page 162 2 Remove the Max Light Cartridge Cell from the cartridge hol...

Страница 167: ...g Leaks Correcting Leaks When If leak has occurred Tools required Description Tissue Preparations Turn the pump off 1 Open the doors 2 Use tissue to dry the leak sensor area 1 Observe the capillary co...

Страница 168: ...System 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 Tubi...

Страница 169: ...C Series Diode Array Detectors User Manual 169 9 Maintenance Replace Leak Handling System Parts 5 Insert the Tubing approximately 85 mm required for replacement between Leak Adapter outlet and Leak Pa...

Страница 170: ...n 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 spec...

Страница 171: ...umber and Firmware Revision The user interface provides module specific information that is stored in the main board These are for example the serial number firmware revision Table 26 RFID Tag Data La...

Страница 172: ...nfinityLab LC Series Diode Array Detectors User Manual 172 10 Parts and Materials for Maintenance Overview of Maintenance Parts 173 Accessory Kit 174 This chapter provides information on parts for mai...

Страница 173: ...tem p n Description 1 5190 0917 Long life Deuterium lamp 8 pin with RFID tag 2 G4212 60008 Max Light Cartridge Cell 10 mm V 1 0 L OR 2 G4212 60007 Max Light Cartridge Cell 60 mm V 4 0 L 2 G7117 60020...

Страница 174: ...5 mm required 5062 8535 Waste accessory kit Flow Cell to waste 5 5067 5737 Door left 6 5067 5736 Door right 7 5043 1013 Tubing Clip Item p n Description p n Description 5062 8535 Waste accessory kit 5...

Страница 175: ...ctors User Manual 175 11 Identifying Cables Cable Overview 176 Analog Cables 178 Remote Cables 180 CAN LAN Cables 183 RS 232 Cables 184 USB Cables 184 This chapter provides information on cables used...

Страница 176: ...Description 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 804...

Страница 177: ...shielded 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 prin...

Страница 178: ...og Cables One end of these cables provides a BNC connector to be connected to Agilent modules The other end depends on the instrument to which connection is being made Agilent Module to 35900 A D conv...

Страница 179: ...ng Cables 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...

Страница 180: ...ension Cable 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...

Страница 181: ...lug Cat5e RJ45 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 G...

Страница 182: ...n 5061 3378 Pin 35900 A D Pin Agilent module Signal Name Active TTL 1 White 1 White Digital ground 2 Brown 2 Brown Prepare run Low 3 Gray 3 Gray Start Low 4 Blue 4 Blue Shut down Low 5 Pink 5 Pink No...

Страница 183: ...o be connected 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 De...

Страница 184: ...32 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 h...

Страница 185: ...the module 190 Information on Instrument Serial Number 190 Interfaces 192 Overview Interfaces 194 ERI Enhanced Remote Interface 196 USB Universal Serial Bus 198 Setting the 6 bit Configuration Switch...

Страница 186: ...properties 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 communica...

Страница 187: ...number 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 numbe...

Страница 188: ...heir initial 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 i...

Страница 189: ...LAN connector 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 t...

Страница 190: ...n on Instrument Serial Number Serial Number Information 1200 Series and 1290 Infinity The serial number information on the instrument labels provide the following information LAN Configuration switch...

Страница 191: ...erial number information on the instrument labels provide the following information CCXZZ00000 Format CC Country of manufacturing DE Germany JP Japan CN China X Alphabetic character A Z used by manufa...

Страница 192: ...32 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 G7132A 2 No Yes Yes 1 A G7161A B 2 Yes Yes No N...

Страница 193: ...quires 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 R...

Страница 194: ...interface replaces the RS 232 Serial interface in new FUSION generation modules For details on USB refer to USB Universal Serial Bus on page 198 Analog Signal Output The analog signal output can be d...

Страница 195: ...V power supply A TTL signal is defined as low or L when between 0 V and 0 8 V and high or H when between 2 0 V and 5 0 V with respect to the ground terminal Table 29 ERI signal distribution Pin Signal...

Страница 196: ...s products using the FUSION core electronics use ERI This interface is already used in the Agilent Universal Interface Box 2 UIB2 ERI Description The ERI interface contains eight individual programmab...

Страница 197: ...rolled 1 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...

Страница 198: ...e Available 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...

Страница 199: ...ctronics Switch settings provide configuration parameters for LAN and instrument specific initialization procedures All modules with FUSION electronics Default is ALL switches DOWN best settings Defau...

Страница 200: ...loaded using update utilities Table 30 6 bit Configuration Switch Mode Function Setting Switch 1 Switch 2 Switch 3 Switch 4 Switch 5 Switch 6 COM1 1 When selecting mode COM settings are stored to non...

Страница 201: ...ule s default parameter May be also required to load main firmware into the module If you use the following switch settings and power the instrument up again it will start as described above CAUTION L...

Страница 202: ...his pack 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 redu...

Страница 203: ...hat maintenance procedures should be scheduled EMF Counters EMF counters increment with use and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is e...

Страница 204: ...et When instrument performance indicates maintenance is necessary take note of the values displayed by the EMF counters Enter these values or values slightly less than the displayed values as EMF limi...

Страница 205: ...r configuration 207 Configuration Switches 208 Initialization Mode Selection 209 Dynamic Host Configuration Protocol DHCP 211 General Information DHCP 211 Setup DHCP 212 Manual Configuration 214 With...

Страница 206: ...ess can be found on a label at the rear of the module underneath the configuration switch see Figure 57 on page 206 Figure 56 MAC Label 2 Connect the instrument s LAN interface see Figure 57 on page 2...

Страница 207: ...ork based 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 212 by manually setting the...

Страница 208: ...figuration Switches The configuration switch can be accessed at the rear of the module Figure 58 Location of Configuration switch example shows a G7114A B VWD The module is shipped with all switches s...

Страница 209: ...ion mode 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 pr...

Страница 210: ...e He may 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...

Страница 211: ...ameters 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...

Страница 212: ...n be found under Details in the LAN section Figure 62 LAN Setting on Instant Pilot 2 Set the configuration switch to DHCP either on the G1369C LAN Interface Card or the mainboard of above mentioned mo...

Страница 213: ...Software e g OpenLAB 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...

Страница 214: ...non volatile 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 beco...

Страница 215: ...lect 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 64 Telnet Starting a session where IP address may be the assigned address...

Страница 216: ...urn 5 Use the and press Enter to list the current settings Table 36 Telnet Commands Value Description displays syntax and descriptions of commands displays current LAN settings ip x x x x sets new ip...

Страница 217: ...toring parameters Figure 69 Closing the Telnet Session Figure 68 Telnet Change IP settings change of IP setting to Initialization mode is Using Stored active TCP IP settings stored TCP IP settings in...

Страница 218: ...Instant Pilot G4208A can be used 1 From the Welcome screen press the More button 2 Select Configure 3 Press the module button of the module that hosts the LAN interface usually the detector 4 Scroll d...

Страница 219: ...trument 221 Do Not Operate in an Explosive Atmosphere 222 Do Not Remove the Instrument Cover 222 Do Not Modify the Instrument 222 In Case of Damage 222 Solvents 223 Safety Symbols 224 Waste Electrical...

Страница 220: ...es 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 ma...

Страница 221: ...compliance 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 224 WARNING Missin...

Страница 222: ...NING Presence 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 th...

Страница 223: ...ompartment For the solvents methanol and ethanol keep the solvent temperature at least 25 C 45 F below the boiling point Do not operate the instrument in an explosive atmosphere Do not use solvents of...

Страница 224: ...warming 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 ser...

Страница 225: ...y from devices and objects that could be damaged by strong magnetic fields Indicates a pinching or crushing hazard Indicates a piercing or cutting hazard Table 37 Symbols WARNING A WARNING alerts you...

Страница 226: ...ment WEEE 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 hou...

Страница 227: ...re 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 assur...

Страница 228: ...ective acids for example lithium iodide potassium chloride and so on high concentrations of inorganic acids like sulfuric acid and nitric acid especially at higher temperatures if your chromatography...

Страница 229: ...de Array Detectors User Manual 229 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...

Страница 230: ...ity II Diode Array Detector FS with fixed slit G7117A Agilent 1290 Infinity II Diode Array Detector with variable slit G7117B and Agilent 1260 Infinity II Diode Array Detector HS with fixed slit G7117...

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