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Agilent 1260 Infinity Refractive Index Detector

1. Autosampler Fu ENX c S 7 E oo T 2 I Sais Thermostat for the ALS optional Solvent cabinet Degasser optional Pump Figure 18 Recommended Two Stack Configuration for 1260 Front View 54 Agilent 1260 Infinity RID User Manual Installing the Refractive Index Detector 3 Optimizing the Stack Configuration LAN to control software CAN Bus cable to Instant Pilot Thermo cable optional Remote cable AC Power CAN Bus cable AC Power Figure 19 Recommended Two Stack Configuration for 1260 Rear View Agilent 1260 Infinity RID User Manual 55 3 Installing the Refractive Index Detector Installing the Detector Parts required Hardware required Preparations Description Power cord For other cables see Cable Overview on page 146 Agilent 1260 Infinity Refractive Index Detector G1362A Locate bench space Provide power connections Unpack the detector The detector is turned on when the line power switch is pressed and the green indicator la
2. Figure 34 Turning the zero glass adjustment screw Agilent 1260 Infinity RID User Manual 125 8 Test Functions Using the Build in Test Chromatogram This function is available from the Agilent ChemStation LabAdvisor and Instant Pilot The built in Test Chromatogram can be used to check the signal path from the detector to the data system and the data analysis or via the analog output to the integrator or data system The chromatogram is continuously repeated until a stop is executed either by means of a stop time or manually The peak height is always the same but the area and the retention time depend on the set peakwidth see examples below 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 LabAdvisor software B 01 03 SP4 or later and open the detector s Tools selection 3 Open the test chromatogram screen Tools Test Chromatogram Current Status Disabled Switch Test Chromatogram on Switch Test Chromatogram att 4 Turn the Test Chromatogram on 5 Change to the detector s Module Service Center and add the detector signal to the Signal Plot window 126 Agilent 1260 Infinity RID User Manual Test Functions 8 Using the Build in Test Chromatogram 6 To start a test chromatogram enter in the
3. 2 Foam not activating the sensor 3 Dirty or defective sensor Agilent 1260 Infinity RID User Manual Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative 105 7 Error Information Cover Violation 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 while the lamps are on or if an attempt is made to switch on for example the lamps with the foam removed the lamps are switched off and the error message is generated Probable cause Suggested actions 1 The top foam was removed during operation Please contact your Agilent service representative 2 Foam not activating the sensor Please contact your Agilent service representative 106 Agilent 1260 Infinity RID User Manual Error Information 7 Refractive Index Detector Specific Error Messages Thermal Fuse Open The thermal fuse of the optical unit heater has failed Probable cause Suggested actions 1 Heater cable disconnected Please contact your Agilent service representative 2 Defective main board Please contact your Agilent service representative 3 Defective thermal fuse Please contact your Agilent service representative Heater Resistance Too High The resistance of the heater foil is above the set limit Probable cause Suggested actions 1 Heater c
4. Agilent Technologies Notices Agilent Technologies Inc 2010 2012 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 61362 90011 Rev B Edition 05 12 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn This product may be used as a com ponent of an in vitro diagnostic sys tem if the system is registered with the appropriate authorities and com plies with the relevant regulations Otherwise it is intended only for gen eral laboratory use Warranty The material contained in this docu ment is provided as is and is sub ject to being changed without notice in future editions Further to the max imum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or perfor mance of this document or of any information contained herein Should Agilent and the user have a separate
5. 88 Agilent 1260 Infinity RID User Manual Agilent 1260 Infinity RID User Manual 6 Troubleshooting and Diagnostics Overview of the Module s Indicators and Test Functions 90 Status Indicators 92 Power Supply Indicator 92 Module Status Indicator 93 User Interfaces 94 Agilent Lab Advisor Software 95 This chapter gives an overview about the troubleshooting and diagnostic features and the different user interfaces ee Agilent Technologies 6 Troubleshooting and Diagnostics Overview of the Module s Indicators and Test Functions Status Indicators The module is provided with two status indicators which indicate the operational state prerun run and error states of the module The status indicators provide a quick visual check of the operation of the module Error Messages In the event of an electronic mechanical or hydraulic failure the module generates an error message in the user interface For each message a short description of the failure a list of probable causes of the problem and a list of suggested actions to fix the problem are provided see chapter Error Information Not Ready Messages During the wait for a specific condition to be reached or completed the detector will generate a not ready message For each message a short description is provided see Not Ready Messages on page 114 Refractive Index Calibration Refractive index calibration is recommended after exchange of the optical unit to
6. Condensation within the module Condensation will damage the system electronics gt Do not store ship or use your module under conditions where temperature fluctuations could cause condensation within the module gt If your module was shipped in cold weather leave it in its box and allow it to warm slowly to room temperature to avoid condensation 42 Agilent 1260 Infinity RID User Manual Site Requirements and Specifications 2 Physical Specifications Table 12 Physical Specifications Type Specification Comments Weight 17 kg 38 Ibs Dimensions height x 180 x 345 x 435 mm 7 x 13 5 x 17 inches width x depth Line voltage 100 240 VAC 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 160 VA 65 W 222 BTU Maximum Ambient operating 0 55 C 32 131 F temperature Ambient non operating 40 70 C 4 158 F temperature Humidity lt 95 at 25 40 C 77 104 F Non condensing Operating Altitude Up to 2000 m 6562 ft Non operating altitude Up to 4600 m 15091 ft For storing the module Safety standards Installation Category II Pollution Degree 2 For indoor use only IEC CSA UL Agilent 1260 Infinity RID User Manual 43 2 Site Requirements and Specifications Performance Specifications 44 Table 13 Performance Specifications Agilent 1260 Infinity Refractive Index Detector Type Specification Comments Detection type Refractive inde
7. Index lamp current toolow 113 lamp voltage too high 112 lamp voltage toolow 112 maximum temperature exceeded 109 not enough light 115 purge time running 114 114 purge valve fuse blown 110 purge valve not connected 111 recycle valve fuse blown 110 recycle valve missing 111 remote timeout 101 thermal fuse open 107 unbalanced diodes 115 undecipherable temperature signal 109 wait for purge 114 wrong temperature profile 108 mobile phase recycling 85 more settings 70 noise 86 non operating altitude 43 non operating temperature 43 not ready message 114 not ready messages not enough light 115 purge time running 114 114 unbalanced diodes 115 wait for purge 114 0 operating Altitude 43 operating temperature 43 optical balance procedure 124 optical unit temperature 84 optical balance 123 optimization check for leaks 84 172 consider solvent changes with time 85 control the optical unit temperature 84 do not overpressurize the flow cell 84 eliminate mobile phase column combination problems 86 flush the degasser 85 position the solvent and waste reservoirs correctly 84 recycle mobile phase 85 use an appropriate response time 85 use the correct solvents 84 verify frit filter and fitting quality 84 P packaging damaged 48 parts identification accessory kit 49 142 parts identification cables 145 parts damaged 48 missing 48 performance specifications 44 physical specifications 43 power supply
8. G1364D FC uS G1367E HiP ALS G1377A HiP micro ALS G2258A DL ALS G4226A ALS 2 Yes Detectors G1314B VWD VL 2 Yes G1314C VWD VL G1314E F VWD 2 No No Yes No No No No No Yes Yes Yes Yes Yes Yes Yes Yes Yes No No No No No Yes Yes Yes CAN DC OUT for CAN slaves Yes THERMOSTAT for G1330B Yes THERMOSTAT for G1330B CAN DC OUT for CAN slaves Yes Yes Yes Agilent 1260 Infinity RID User Manual 25 1 Introduction to the Refractive Index Detector Table 1 Agilent 1200 Infinity Series Interfaces Module CAN LAN BCD LAN RS 232 Analog APG Special optional on board Remote G4212A B DAD 2 No Yes Yes 1 Yes G1315C DAD VL 2 No Yes Yes 2 Yes G1365C MWD G1315D DAD VL G1365D MWD VL G1321B FLD 2 Yes No Yes 1 Yes G1362A RID G4280A ELSD No No No Yes Yes Yes EXT Contact AUTOZERO Others G1316A C TCC 2 No No Yes No Yes G1322A DEG No No No No No Yes AUX G1379B DEG No No No Yes No No AUX G4227A Flex Cube 2 No No No No No G4240A CHIP CUBE 2 Yes No Yes No Yes CAN DC OUT for CAN slaves THERMOSTAT for G1330A B NOT USED 26 The detector DAD MWD FLD VWD RID is the preferred access point for control via LAN The inter module communication is done via CAN e CAN connectors as interface to other modules e LAN connector as interface to the control software e RS 232C as interface to a computer e REMOTE connector as interface to other
9. Purge Valve on Purge Valve off b RID Tools screen via Tools If an Agilent pump is part of the system the pump section is active Agilent 1260 Infinity RID User Manual 119 Test Functions Refractive Index Calibration Tools RID Tool Screen mM Reference Cell No pump available Pump FP Use Pump Purge Time min 4 Purge Flow ml min Solvent Channel Purge Reference Cell Last Purge 2010 01 22 10 23 42 m Recycle Valve Waste Recycle m Optical Balance Off 0 1 000 On 1 000 Diode Balance c RID Calibration screen via Calibrations Test Name Refractive Index Calibration Description This procedure performs a refractive index calibration Module G13624 DE 91600336 Approx Time 1 min Status Running m Test Procedure a gt 1 Check pre condition Purge of reference cell Switch recycle valve to Waste c Refractive Index Calibration Fil conwalstonard Pre condition is to have the sample and reference cell purged with HPLC grade water Are the cells already purged with water If not the RID Tools screen offers the Purge Reference Cell tool to Fulfill this task Press OK if pre condition is fulfilled Cancel otherwise Verify calibration data ne wv N Calibrate refractive index Use the functions as described in the steps below 4 Flushing the degasser and pump 120 Agilent 1260
10. h Remove all blanking plugs from all outlet ports waste amp recycle of the detector to avoid potential damage to the flow cell if the recycle valve is accidentally switched to one of these ports while flow is applied to the detector 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 Route the tubing behind the front covers of the modules in the stack 6 Direct the waste tube into a suitable waste container Make sure that there is no restriction of this tube 7 If solvent recycling is to be used direct the recycle tube into the solvent bottle Make sure that there is no restriction of this tube 8 Establish flow and observe if leaks occur Agilent 1260 Infinity RID User Manual 61 3 Installing the Refractive Index Detector Flow Connections 9 Replace the front cover The installation of the detector is now complete 62 Agilent 1260 Infinity RID User Manual Agilent 1260 Infinity RID User Manual ee 4 Using the Refractive Index Detector e i e j Operation of the Refractive Index Detector 64 Before Using the System 64 Refractive Index Detector Control 66 Refractive Index Detector Settings 68 Refractive Index Detector More Settings 70 Runnin
11. 0 2 min 4 s standare x Timetable Line Time Polarity Peakwidth Jeet Append Cut a z bekk Cancel Help Figure 23 Refractive Index Detector Settings Optical Unit Temperature This item sets the temperature of the optical unit The optical unit of the Agilent 1260 Infinity RID can be operated between 5 C above ambient and 55 C The recommended setting is 5 C above ambient This will improve baseline stability e Polarity This item sets the polarity of the RID signal Because of the nature of analytes and eluents refractive index detectors can show negative and positive peaks even within a run Select the Signal Polarity you expect from your data from Negative or Positive Agilent 1260 Infinity RID User Manual Using the Refractive Index Detector 4 e Automatic Recycling This parameter can be used to select between automatic recycling of the eluent on or directing the eluent to the waste outlet of the RID off after the run Time Stoptime Stoptime enables you to set a time at which the RID stops an analysis If the RID is used with other Agilent 1200 Infinity Series modules the RID stoptime stops the RID only and does not stop any other modules Limits 0 00 to 99999 00 minutes asPump the stoptime of the pump when an Agilent pump is configured asInj the stoptime of the injector if an Agilent 1200 Infinity Series injector but no Agilent pump is configured or noLimit an infinite run
12. 2 m 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 s also called Null Modem Cable with full handshaking where the wiring is made between pins 1 1 2 3 3 2 4 6 5 5 6 4 7 8 8 7 9 9 RS 232 cable 8m Agilent 1260 Infinity RID User Manual 147 11 Identifying Cables Analog Cables o 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 3394 6 Integrators p n 35900 60750 Pin 3394 6 Pin Agilent Signal Name module 1 Not connected 2 Shield Analog 3 Center Analog 148 Agilent 1260 Infinity RID User Manual Agilent Module to BNC Connector Identifying Cables 11 p n 8120 1840 Pin BNC Pin Agilent Signal Name module ar Shield Shield Analog i Center Center Analog Agilent Module to General Purpose p n 01046 60105 Pin 3394 6 Pin Agilent Signal Name module 1 Not connected 2 Black Analog Analog Pe i 3 Red eo Agilent 1260 Infinity RID User Manual 149 11 Identifying Cables Remote Cables 150 One end of these cables provides a Agilent Technologies APG Analytical Products Group remote connector to be connected to Agilent modules The other end depends on the instrument to be con
13. Bootp mode for LAN e for boot test modes DIPS 1 2 must be UP plus required mode Switch settings provide configuration parameters for GPIB address serial communication protocol and instrument specific initialization procedures With the introduction of the Agilent 1260 Infinity all GPIB interfaces have been removed The preferred communication is LAN The following tables represent the configuration switch settings for the modules without on board LAN only Agilent 1260 Infinity RID User Manual 33 1 34 Introduction to the Refractive Index Detector Table 5 8 bit Configuration Switch without on board LAN Mode Select 1 2 3 4 5 6 7 8 RS 232C 0 1 Baudrate Data Parity Bits Reserved 1 0 Reserved TEST BOOT 1 1 rsvo sys rsvo Rsvo Fc The LAN settings are done on the LAN Interface Card G1369A B Refer to the documentation provided with the card Communication Settings for RS 232C The communication protocol used in the column compartment supports only hardware handshake CTS RTR Switches 1 in down and 2 in up position define that the RS 232C parameters will be changed Once the change has been completed the column instrument must be powered up again in order to store the values in the non volatile memory Table6 Communication Settings for RS 232C Communication without on board LAN Mode Select 1 2 3 4 5 6 7 8 RS 232C 0 1 Baudrate Data Bits Parity Use the following tables for s
14. required co Close the service door 6 Replace the front cover Valves and tubing Service door Leak sensor Figure 36 Observing for Leaks 136 Agilent 1260 Infinity RID User Manual Maintenance Replacing Leak Handling System Parts Replacing Leak Handling System Parts When If the parts are corroded or broken Parts required p n Description 1 5061 8388 Leak funnel 1 5041 8389 Leak funnel holder 1 5042 9974 Tubing Flex 1 5 m Leak tubing 120 mm required 1 Remove the front cover 2 Pull the leak funnel out of the leak funnel holder 3 Pull out the leak funnel with the tubing 4 Insert the leak funnel with the tubing in its position 5 Insert the leak funnel into the leak funnel holder 6 Replace the front cover Leak funnel holder Leak funnel J p ai ST l D N i Eg Leak tubing y Ih r A Leak sensor E i L Ael S a o gt OD E Figure 37 Replacing Leak Handling System Parts Agilent 1260 Infinity RID User Manual 137 9 Maintenance Replacing the Detector s Firmware When Tools required Parts required Preparations 138 The installation of newer firmware might be necessary if a newer version solves problems of older versions or to keep all systems on the same validated revision The installation of older firmwar
15. 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 Agilent 1260 Infinity RID User Manual 151 11 Identifying Cables Agilent Module to General Purpose p n 01046 60201 Pin Universal Pin Agilent Signal Name Active module TTL 1 White Digital ground A Q 1 2 B ou Brown Prepare run Low 00 pees DE KEY 3 Gray Start Low oo T oo z EE te 4 aa Shut down Low og 5 Pink Not connected oo 26 6 Yellow Power on High 5 15 7 Red Ready High 8 Green Stop Low 9 Black Start request Low 152 Agilent 1260 Infinity RID User Manual BCD Cables Identifying Cables 11 One end of these cables provides a 15 pin BCD connector to be connected to the Agilent modules The other end depends on the instrument to be connected to Agilent Module to General Purpose p n G1351 81600 Wire Color Pin Agilent Signal Name BCD Digit module Green 1 BCD 5 20 Violet 2 BCD 7 80 a Blue 3 BCD 6 40 m Yellow 4 BCD 4 10 SS Black 5 BCD 0 1 Ras Orange 6 BCD 3 8 Red 7 BCD 2 4 Brown 8 BCD 1 2 Gray 9 Digital ground Gray Gray pink 10 BCD 11 800 Red blue 11 BCD 10 400 White green 12 BCD 9 200 Brown green 13 BCD 8 100 notconnected 14 notconnected 15 5V Low Agilent 1260 Infinity RID User Manual 153 11 Identifying Cables Agilent Mo
16. Agilent products e Analog output connector s for signal output Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 Overview Interfaces CAN The CAN is inter module communication interface It is a 2 wire serial bus system supporting high speed data communication and real time requirement LAN The modules have either an interface slot for an LAN card e g Agilent G1369A B LAN Interface or they have an on board LAN interface e g detectors G1315C D DAD and G1365C D MWD This interface allows the control of the module system via a connected PC with the appropriate control software If an Agilent detector DAD MWD FLD VWD RID is in the system the LAN should be connected to the DAD MWD FLD VWD RID due to higher data load If no Agilent detector is part of the system the LAN interface should be installed in the pump or autosampler RS 232C Serial The RS 232C connector is used to control the module from a computer through RS 232C connection using the appropriate software This connector can be configured with the configuration switch module at the rear of the module Refer to Communication Settings for RS 232C There is no configuration possible on main boards with on board LAN These are pre configured for e 19200 baud 8 data bit with no parity and one start bit and one stop bit are always used not selectable The RS 232C is designed as DCE data communication equipment
17. CAUTION Safety standards for external equipment gt If you connect external equipment to the instrument make sure that you only use accessory units tested and approved according to the safety standards appropriate for the type of external equipment 132 Agilent 1260 Infinity RID User Manual Maintenance 9 Detector Maintenance Procedures On the following pages maintenenance procedures are described that can be carried out without opening the main cover Table 18 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 If broken or corroded Check for leaks replacement Replacing the detector s If not up to date or corrupted Firmware Agilent 1260 Infinity RID User Manual 133 9 Maintenance Cleaning the Module The module case should be kept clean Cleaning should be done with a soft cloth slightly dampened with water or a solution of water and mild detergent Do not use an excessively damp cloth as liquid may drip into the module WARNING Liquid dripping into the electronic compartment of your module Liquid in the module electronics can cause shock hazard and damage the module gt Do not use an excessively damp cloth during cleaning gt Drain all solvent lines before opening any fittings 134 Agilent 1260 Infinity RID User Manual Maintenance 9 Flow Cell Flushi
18. Figure 38 Location of the Interface Board Agilent 1260 Infinity RID User Manual 139 9 Maintenance Replacing the Interface Board 140 Agilent 1260 Infinity RID User Manual Agilent 1260 Infinity RID User Manual e e e a M L o ee 10 9209 Parts for Maintenance i nail j Accessory Kits 142 This chapter provides information on parts for maintenance 141 Agilent Technologies 10 Parts for Maintenance Accessory Kits 142 Accessory kit p n G1362 68755 contains some accessories needed for the installation of the detector p n Description G1362 68706 Interface tubing kit G1362 87300 Interfacing capillary G1362 87301 Restriction capillary 5181 1516 CAN cable Agilent module to module 0 5 m 0100 1847 PEEK adapter 1 4 28 to 10 32 Adapter AIV to solvent inlet tubes peee e E om Figure 39 Interface Tubing Kit Parts S gt __ _ S SS Figure 40 Interfacing Capillary Parts Agilent 1260 Infinity RID User Manual Parts for Maintenance 10 Accessory Kits Figure 41 Restriction Capillary Parts Agilent 1260 Infinity RID User Manual 143 10 Parts for Maintenance Accessory Kits 144 Agilent 1260 Infinity RID User Manual Agilent 1260 Infinity RID User Manual 11 Identifying Cables Cable Overview 146 Analog Cables 148 Remote Cables 150 BCD Cables 153 CAN LAN Cables 155 Agilent Module to PC 156 External Contact Cable 157 This chapter provides information on cables used with t
19. Index Detector Unpacking the Detector 48 Delivery Checklist 48 Optimizing the Stack Configuration 51 Optimizing the One Stack Configuration 52 Optimizing the Two Stack Configuration 54 Installing the Detector 56 Flow Connections 59 This chapter provides information on unpacking checking on completeness stack considerations and installation of the detector ott Agilent Technologies 47 3 Installing the Refractive Index Detector Unpacking the Detector CAUTION If the delivery packaging shows signs of external damage please call your Agilent Technologies sales and service office immediately Inform your service representative that the instrument may have been damaged during shipment Defective on arrival problems If there are signs of damage please do not attempt to install the module Inspection by Agilent is required to evaluate if the instrument is in good condition or damaged gt Notify your Agilent sales and service office about the damage gt An Agilent service representative will inspect the instrument at your site and initiate appropriate actions Delivery Checklist 48 Delivery Checklist Ensure all parts and materials have been delivered with your module The delivery checklist is shown below For parts identification please check the illustrated parts breakdown in Parts for Maintenance on page 141 Please report any missing or damaged parts to your local Agilent Technologies sales and s
20. Infinity RID User Manual Test Functions 8 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 you click continue 6 Fill the sample cell with calibration solution Remove the inlet capillary or flushing syringe from the in port Take the syringe and fix the needle to the syringe adapter Keep the syringe in a horizontal position a b c Suck about 1 5 mL of the calibration sample into the syringe d e Remove the needle f Add the filter to the syringe and fit the needle to filter Sample filter Figure 33 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 Do not inject the calibration solution without the sample filter i Slowly inject about 1 0 ml and wait for about 10 s to inject another 0 1 mL This will assure that the cell is filled properly Agilent 1260 Infinity RID User Manual 121 122 Test Functions 7 Calibrate refractive index a Ifthe detector response differs from the theoretical response of 512 000 nRIU 5 000
21. Introduction to the Refractive Index Detector 1 Early Maintenance Feedback Maintenance requires the exchange of components which are subject to wear or stress Ideally the frequency at which components are exchanged should be based on the intensity of usage of the detector and the analytical conditions and not on a predefined time interval The early maintenance feedback EMF feature monitors the usage of specific components in the instrument and provides feedback when the user selectable limits have been exceeded The visual feedback in the user interface provides an indication that maintenance procedures should be scheduled EMF Counters The detector provides one EMF counter for the reference liquid age The counter increments with the time that liquid remains in the reference cell and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded The counter is reset to zero after the reference cell is purged Using the EMF Counters The user selectable EMF limits for the EMF counters enable the early maintenance feedback to be adapted to specific user requirements The useful counter time since last purge is dependent on the requirements for the analysis therefore the definition of the maximum limits need to be determined based on the specific operating conditions of the instrument Setting the EMF Limits The setting of the EMF limits must be optimized over one or two maintenan
22. RID p n Description 1 61362 87301 Restriction capillary 1 Turn ON the detector You are now ready to change the settings of your detector 2 Connect the restriction capillary directly between the column compartment heat exchanger outlet and the in port of the detector 3 Set up the instrument with the following test conditions Table 17 Chromatographic Conditions Mobile phases LC grade water Column Restriction capillary 2 7 m x 0 17 mm i d Flow rate 1 0 ml min Compressibility 46 Stroke 20 pl Stop time 20 min Column compartment temperature 40 C Optical unit Temperature 40 C Polarity Positive Peak Width Response time 0 2 min 4 s standard Agilent 1260 Infinity RID User Manual Using the Refractive Index Detector 4 Checking Baseline Noise and Drift 4 Set the RID setpoints according to Figure 28 on page 77 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 RID Signal Instrument 2 koo S R Figure 28 RID Baseline Check Parameters NOTE The Agilent ChemStation can automatically calculate the baseline short term noise long term noise wander and drift Follow steps 4 to 9 NOTE If you are not using the Agilent ChemStation go to step 10 5 Edit the Agilent ChemStation method Agilent 1260 Infinity RID
23. User Manual 77 4 Using the Refractive Index Detector 6 Specify the report style Performance Noise as shown in Figure 29 on page 78 Specify Report Instrument 2 x Destination Quantitative Results E H l Screen Calculate Percent M File Type Based On Area gt x Fil tie K IxT D WMF File Prefix cme r y Sorted By Signal gt No1s2 C xs C HTM Signal Options Style Report Style Performance Noise M l Sample info on each page x Add Chromatogram Output l Add Summed Peaks Table Report Layout For Uncalibrated Peaks C Separately With Calibrated Peaks C Do Not Report Chromatogram Output f Size Portrait of Page C Landscape Time zs C Multi Page Landscape z5 Response 30 Wz Pages Figure 29 RID Baseline Check Out Report 78 Agilent 1260 Infinity RID User Manual Using the Refractive Index Detector Checking Baseline Noise and Drift 7 Set the noise determination time range to 0 20 minutes as shown in Figure 30 on page 79 Noise Determination Instrument 2 U E E E __ __ __ EE ma Figure 30 RID Baseline Check Out Noise Ranges 8 Save the Agilent ChemStation method Agilent 1260 Infinity RID User Manual 4 79 4 Using the Refractive Index Detector Checking Baseline Noise and Drift 9 Turn the heater ON and purge the detector reference cell for 20 minutes as shown in Figure 31 on page 80 R
24. a skilled person who is aware of the hazard involved Do not attempt internal service or adjustment unless another person capable of rendering first aid and resuscitation is present Do not replace components with power cable connected Do not operate the instrument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or make any unauthorized modification to the instrument Capacitors inside the instrument may still be charged even though the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious personal injury are present in this instrument Use extreme caution when handling testing and adjusting When working with solvents please observe appropriate safety procedures e g goggles safety gloves and protective clothing as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used Agilent 1260 Infinity RID User Manual Appendix 12 The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC Abstract The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC adopted by EU Commission on 13 February 2003 is introducing producer responsibility on all Electric and Electronic appliances from 13 August 2005 s This product complies with the WEEE D
25. command line STRT Set heater temperature 35 Send Generic command line stor 7 Send A Signal configuration Available signals Signal A mA G13 x Add Select signal Signal A RIU G13 7 Remove IV Autoscroll Generic plot RA 0000 STAT G13624 DE91600336 5 4 2010 3 19 20 PM RA 0000 STOP G13624 DE91600336 5 4 2010 3 24 11 PM Time min Figure 35 Test Chromatogram with Agilent LabAdvisor 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 Agilent 1260 Infinity RID User Manual 127 8 Test Functions Using the Build in Test Chromatogram 128 Agilent 1260 Infinity RID User Manual This chapter provides general information on maintenance of the detector Agilent 1260 Infinity RID User Manual 9 Maintenance Introduction to Maintenance 130 Warnings and Cautions 131 Detector Maintenance Procedures 133 Cleaning the Module 134 Flow Cell Flushing 135 Correcting Leaks 136 Replacing Leak Handling System Parts 137 Replacing the Detector s Firmware 138 Replacing the Interface Board 139 ee Agilent Technologies 129 9 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 stack There are no serviceable parts inside Do not open the module 130 Agilent 1260 Infinity RID User Manual Maintenan
26. ensure correct operation of the detector The procedure uses a solution of known refractive index compared to LC grade water see Refractive Index Calibration on page 118 90 Agilent 1260 Infinity RID User Manual Troubleshooting and Diagnostics 6 Optical Balance Optical balance allows the balance of light falling on the light receiving diodes to be restored The sample and reference cells must both be fully purged before the procedure is started see Optical Balance on page 123 Agilent 1260 Infinity RID User Manual 91 6 Troubleshooting and Diagnostics Status Indicators Two status indicators are located on the front of the module The lower left indicates the power supply status the upper right indicates the module status Status indicator 7 o Line power switch with green light Power Supply Indicator The power supply indicator is integrated into the main power switch When the indicator is illuminated green the power is ON 92 Agilent 1260 Infinity RID User Manual Troubleshooting and Diagnostics 6 Module Status Indicator The module status indicator indicates one of six possible module conditions e When the status indicator is OFF and power switch light is on the module is in a prerun condition and is ready to begin an analysis e A green status indicator indicates the module is performing an analysis run mode e A yellow indicator indicates a not ready con
27. flowing will ensure that the liquid in the reference cell is as similar as possible to the flowing solvent The purge valve can be manually set to the on position for a defined time or the Automatic purge mode can be enabled In this mode the purge valve will automatically switch to the ON position for a defined purgetime prior to the start of each analysis If a purgetime is set then a waittime must also be set to allow the detector baseline to stabilize after the switching of the purge valve position After both the purgetime and waittime have been completed the analysis will start If the Automatic zero before analysis mode is enabled the detector output will be set to zero immediately before the analysis begins Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 2 gt Flow path with purge valve on Flow path with purge valve off Figure 5 Flow Path 1 1 Flow in 2 Heater 3 Heat exchanger 4 Sample cell 5 Purge valve Recycle valve 7 Waste container 8 Reference cell 9 Solvent bottle Agilent 1260 Infinity RID User Manual 17 1 Introduction to the Refractive Index Detector COM COMMON from optical unit to optical unit NO NORMALLY OPEN sample cell top right sample cell bottom right NC NORMALLY CLOSED 1 Purge valve Recycle valve CONNECTINGPORTS RECYCLE top left bottom left optical unit from and to reference cell
28. for solvent degassing Remote Timeout Suggested actions Fix the leak in the external instrument before restarting the module Check external instruments for a shut down condition Check the vacuum degasser for an error condition Refer to the Service Manual for the degasser or the 1260 pump that has the degasser built in A not ready condition is still present on the remote input When an analysis is started the system expects all not ready conditions for example a not ready condition during detector balance to switch to run conditions within one minute of starting the analysis If a not ready condition is still present on the remote line after one minute the error message is generated Probable cause 1 Not ready condition in one of the instruments connected to the remote line 2 Defective remote cable 3 Defective components in the instrument showing the not ready condition Agilent 1260 Infinity RID User Manual Suggested actions Ensure the instrument showing the not ready condition is installed correctly and is set up correctly for analysis Exchange the remote cable Check the instrument for defects refer to the instrument s documentation 101 7 102 Error Information Synchronization Lost Leak During an analysis the internal synchronization or communication between one or more of the modules in the system has failed The system processors continually monitor the system configuration
29. indicator 92 power consideration 40 power consumption 43 power cords 41 radio interference 165 refractive index calibration procedure 118 refractive index detector optimization 64 refractive index detector optimization 84 refractive index calibration 118 refractive index calibration 118 optical balance 123 remote cable 150 repairs cautions and warnings 131 correction leaks 136 flow cell flushing 135 replacing interface board BCD LAN 139 replacing leak handling system 137 replacing firmware 138 138 response time 85 restriction capillary 86 RS 232C cable 156 communication settings 34 S safety class 161 safety information lithium batteries 164 safety general information 161 standards 43 symbols 160 serial number information 24 settings 68 shut down 101 site requirements 39 power cords 41 solvent and waste reservoirs 84 Solvent Information 64 solvent information 167 solvents 84 85 167 sound emission 166 Agilent 1260 Infinity RID User Manual Index special interfaces 30 Vv special settings i voltage range 43 boot resident 36 tored cold start 36 W specification physical 43 wander 86 specifications warnings and cautions 131 analog outputs 45 weight 43 communications 45 GLP features 45 performance 44 safety and maintenance 45 stack configuration front view 52 rearview 50 status indicator 93 synchronization lost 102 T temperature sensor 102 test chromatogram 126 tests tes
30. nRIU enter the theoretical value 512 000 in the dialog box If the detector response is within the theoretical response click OK 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 Agilent 1260 Infinity RID User Manual Test Functions 8 Optical Balance Optical Balance When the sample and reference cells both contain the same liquids an equal amount of light should fall on each light receiving diode the diode balance will equal 0 If this balance of light needs to be corrected the optical balance procedure can be used Diode balance is calculated as follows diode diode diode diode diode balance Where diode signal proportional to the amount of light falling on diode e diodes signal proportional to the amount of light falling on diodes 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 The detector will become not ready when the diode balance value falls outside the range 0 5 to 0 5 Both sample and reference cell must be purged with the same solvent before optical balance is performed Prior to performing this procedure the system must be well equilibrated Agilent 1260 Infinity RID User Manual 12
31. s Physical Specifications 43 Performance Specifications 44 This chapter provides information on environmental requirements physical and performance specifications oe Agilent Technologies 39 2 Site Requirements and Specifications Site Requirements A suitable environment is important to ensure optimal performance of the instrument Power Considerations The module power supply has wide ranging capability It accepts any line voltage in the range described in Table 12 on page 43 Consequently there is no voltage selector in the rear of the module There are also no externally accessible fuses because automatic electronic fuses are implemented in the power supply Hazard of electrical shock or damage of your instrumentation can result if the devices are connected to a line voltage higher than specified gt Connect your instrument to the specified line voltage only Module is partially energized when switched off as long as the power cord is plugged in Repair work at the module can lead to personal injuries e g electrical shock when the cover is opened and the module is connected to power gt Always unplug the power cable before opening the cover gt Do not connect the power cable to the instrument while the covers are removed CAUTION Unaccessable power plug In case of emergency it must be possible to disconnect the instrument from the power line at any time gt Make sure the power connector o
32. time The stoptime setting depends on the configured pump If you have an Agilent pump with an Agilent injector then the pump is the stoptime master asPump If you have a non Agilent pump and an Agilent 1200 Infintiy Series injector then the injector is the stoptime master asInj Posttime You can set the Posttime so that your RID remains in the not ready state during the Posttime to delay the start of the next analysis A Posttime period can be used to allow your column to equilibrate after changes in solvent composition Limits 0 to 99999 00 minutes or Off Off sets the posttime to 0 0 min e Peakwidth Peakwidth enables you to select the peak width response time for your analysis The peak width is defined as the width of a peak in minutes at half the peak height Set the peak width to the narrowest expected peak in your chromatogram The peak width sets the optimum response time for your RID Limits When you set the peak width in minutes the corresponding response time is set automatically and the appropriate data rate for signal acquisition is selected please refer to the ChemStation s Online help for more details Agilent 1260 Infinity RID User Manual 69 4 Using the Refractive Index Detector Refractive Index Detector More Settings The following operating instructions were generated using the Agilent B 01 03 ChemStation as operating software How To Get There The RID Signal dialog box is displayed when you se
33. written agreement with warranty terms covering the material in this document that conflict with these terms the warranty terms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcon tract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or asa commercial item as defined in FAR 2 101 a or as Restricted computer soft ware as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or dis closure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly per formed or adhered to could result in
34. 1 Defective main board Please contact your Agilent service representative 2 Defective heater Please contact your Agilent service representative Agilent 1260 Infinity RID User Manual 109 7 Error Information Purge Valve Fuse Blown The electronic fuse on the purge valve has 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 representative 3 Defective main board Please contact your Agilent service representative Recycle Valve Fuse Blown The electronic fuse on the recycle valve has been activated Probable cause Suggested actions 1 Short in recycle valve circuit Power cycle the module 2 Defective recycle valve Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative 110 Agilent 1260 Infinity RID User Manual Error Information 7 Purge Valve Not Connected When activated no response was received from the purge valve Probable cause Suggested actions 1 Purge valve disconnected Please contact your Agilent service representative 2 Defective purge valve Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative Recycle Valve Missing When activated no response was received from the recycle valve Probable cause Suggested actions 1 Recycle valve di
35. 3 8 Test Functions The Optical Balance Procedure When When light falling on light receiving diodes is out of balance Tools required e Flat head screwdriver This procedure should only be performed to correct a permanent misalignment of the light beam that cannot be eliminated by flushing the sample and the reference cell with the same solvent and by equilibrating the system 1 Purging the sample and reference cells a 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 2 Start optical balance a Using the Agilent LabAdvisor Software B 01 03 SP3 or later open the RID Tools screen Tools RID Tool Screen m Reference Cell No pump available m Pump I Use Pump Purge Time min 1 Purge Flow ml min Solvent Channel Purge Reference Cell m Recycle Valve Last Purge 2010 01 22 10 23 42 Waste Recycle Optical Balance Off C on 1 000 0 1 000 Diode Balance 124 Agilent 1260 Infinity RID User Manual Test Functions 8 Optical Balance 3 Adjust optical balance a While monitoring the optical balance use the flat headed screwdriver to turn the zero glass adjustment screw slowly see Figure 34 on page 125 b When the diode balance value reaches 0 00 optical balance is restored Zero glass adjustment screw left
36. Check Out Sample Control 5 When purging has finished allow the baseline to stabilize and start the analysis 74 Agilent 1260 Infinity RID User Manual Using the Refractive Index Detector 4 The resulting chromatogram is shown in the figure below RID1 A RID A Refractive Index Signal RIDTES T RIDO0011 0 Figure 27 Isocratic Standard Sample Chromatogram 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 nothing more 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 expected ina regular chromatogram especially if a non degassed sample is injected into degassed solvent and the sample solvent properties don t perfectly match with the mobile phase properties Only similar zooming factors in the display of a chromatogram will lead to similar looking results Agilent 1260 Infinity RID User Manual 75 4 Using the Refractive Index Detector Checking Baseline Noise and Drift Setting the Test Conditions When Tools required Parts required 76 This chapter describes checking the baseline noise and drift for the Agilent 1260 Infinity Refractive Index Detector If you want to checkout the detector LC system with G1362A
37. F 168 Agilent 1260 Infinity RID User Manual Appendix 12 Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com Select Products Chemical Analysis It will provide also the latest firmware of the modules for download Agilent 1260 Infinity RID User Manual 169 Index Index 8 bit configuration switch on board LAN 31 without On Board LAN 33 A accessory kit parts 49 142 Agilent Diagnostic software 95 Agilent Lab Advisor software 95 Agilent Lab Advisor 95 Agilent oninternet 169 algae 167 167 algea 135 ambient operating temperature 43 ambient non operating temperature 43 analog signal 28 analog cable 148 apgremote 29 ASTM environmental conditions 42 automatic recycling after analysis 16 automatic zero before analysis 16 automatic purge 16 balance 91 baseline noise and drift 76 baseline noise 86 baseline drift 86 equilibration 87 170 noise 86 wander 86 battery safety information 164 BCD cable 153 bench space 42 C cable analog 148 BCD 153 CAN 155 connecting APG remote 55 connecting CAN 55 connecting GPIB 55 connecting LAN 55 connecting the ChemStation 55 connecting the power 55 external contact 157 LAN 155 remote 150 RS 232 156 cables analog 146 BCD 146 CAN 147 LAN 147 overview 146 remote 146 RS 232 147 calibration 90 refractive index 90 CAN cable 155 cauti
38. Figure 6 G1362A Physical Plumbing Connections 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 reference valve are made of PTFE available as Tubing kit p n G1362 68709 18 Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector Purge valve Recycle valve Metal union block COM COMMON NO NORMALLY OPEN NC NORMALLY CLOSED Reference cell Figure 7 Flow path with the Purge and Recycle Valves OFF 1 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 Agilent 1260 Infinity RID User Manual 19 1 Introduction to the Refractive Index Detector Flow Path Purge valve Recycle valve Metal union block Sample cell COM COMMON RECYCLE WASTE NO NORMALLY OPEN COM NORMALLY CLOSED Reference cell Figure 8 Flow path with the Purge and Recycle Valves ON 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 20 Agilent 1260 Infinity RID User Manual
39. ID Control Instrument 2 Figure 31 RID Baseline Check Control 10 When purging has finished allow the baseline to stabilize and start the sequence blank run no injection 80 Agilent 1260 Infinity RID User Manual Using the Refractive Index Detector 4 i i Checking Baseline Noise and Drift 11 The Agilent ChemStation report is shown in Figure 32 on page 81 H OQNOIS2 c Notepad Biel es File Edit Search Help Injection Date 3 31 03 2 16 28 PM Sample Name NOIS 1 Location Acq Operator Inj D HPCHEM 2 SEQUENCE OQPU OQNOIS2 D HPCHEM 2 METHODS OQPU OQNOIS2 M 8 21 01 10 36 51 AM Signal 1 RID1 A Refractive Index Signal Results obtained with enhanced integrator Noise determination Time range Noise Noise Noise from to 6 SD PtoP ASTM Wander Drift min min nRIU nRIU nRIU nRIV nRIU h Sr meas ee pata ae FS See eS 0 000 20 000 14 5484 12 6403 3 2124 7 8886 19 639 xxx End of Report xxx Figure 32 Baseline Check Out Results Agilent 1260 Infinity RID User Manual 81 4 82 Using the Refractive Index Detector Evaluation For the Instant Pilot Rescale the plot and measure the baseline noise and drift on the screen If a printer is configured for the instrument the plot can be printed by pressing the m key and selecting Print Plot The following values are calculated automatically by the Agilent ChemStation Noise ASTM The short term noise in nRIU b
40. 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 CAN cable disconnected Ensure all the CAN cables are connected correctly Ensure all CAN cables are installed correctly 2 Defective CAN cable Exchange the CAN cable 3 Defective main board in another module Switch off the system Restart the system and determine which module or modules are not recognized by the system A leak was detected in the module The signals from the two temperature sensors leak sensor and board mounted temperature compensation sensor are used by the leak algorithm to determine whether a leak is present When a leak occurs the leak sensor is cooled by the solvent This changes the resistance of the leak sensor which is sensed by the leak sensor circuit on the main board Probable cause Suggested actions 1 Loose fittings Ensure all fittings are tight 2 Broken capillary Exchange defective capillaries 3 Leaking valve Exchange valve 4 Leaking flow cell Exchange flow cell Agilent 1260 Infinity RID User Manual Error Information 7 Leak Sensor Open The leak sensor in the module has failed open circuit The current through the leak sensor is dependent on temperature A leak is detected when solvent cools the leak sensor causing the leak sensor current to change within defined limits If the current falls outside the lower limit the
41. Method J7 Take current method Analog Output Range Con ioff Cow cy Purge Reference Cell p At Power On on off 2 M Turn heater on forf20 0 Sfrrin Automatic Turn On I Tum heater on at mjd Hhimms Cancel Help Figure 22 Refractive Index Detector Control Heater Select the on option to switch the RID heater on This parameter requires to set the Optical Unit Temperature Select the off option to switch the optical unit heater off Error Method The Error Method group enables you to select the method that is run when an error occurs It ensures that the instrument shuts down in a controlled manner if the ChemStation control is discontinued for any reason When Take current method is checked the current method is copied to the module and stored if an error occurs the module will run the stored method e 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 Agilent 1260 Infinity RID User Manual Using the Refractive Index Detector 4 Analog Output Range The Analog Output Range group allows you to select the voltage ranges of the analog output of the refractive index detector Select 0 1 V to set the full scale output to 0 1 volts Select 1 V to set the full scale output to 1 volt Purge Reference Cell This parameter is used to exchange the content of the reference ce
42. S 232C APG Remote ready start stop and shut down signals Extensive diagnostics error detection and display through control module and ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas Early maintenance feedback EMF for continuous tracking of instrument usage with user selectable limits and feedback messages Electronic records of maintenance and errors Automated operational qualification performance verification 0O PV All materials recyclable Agilent 1260 Infinity RID User Manual 45 2 46 Site Requirements and Specifications Table 13 Performance Specifications Agilent 1260 Infinity Refractive Index Detector Type Specification Comments Environment 0 to 55 C constant temperature at lt 95 humidity non condensing Dimensions 180 mm x 345 mm x 435 mm 7 x 13 5 x 17 inches height x width x depth Weight 17 kg 38 Ibs 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 compartment temperature 35 C Agilent on line degasser G1322A pump and thermostatted column compartment Instrument equilibrated for 2 hours Agilent 1260 Infinity RID User Manual Agilent 1260 Infinity RID User Manual 3 Installing the Refractive
43. Sensor Short The ambient compensation sensor NTC on the main board in the module has failed short circuit The resistance across the temperature compensation sensor NTC on the main board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor falls below the lower limit the error message is generated Probable cause Suggested actions 1 Defective main board Please contact your Agilent service representative Agilent 1260 Infinity RID User Manual Fan Failed Error Information 7 The cooling fan in the module has failed The hall sensor on the fan shaft is used by the main board to monitor the fan speed If the fan speed falls below a certain limit for a certain length of time the error message is generated This limit is given by 2 revolutions second for longer than 5 seconds Probable cause 1 Fan cable disconnected 2 Defective fan 3 Defective main board Open Cover The top foam has been removed Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative 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 1 The top foam was removed during operation
44. This is a Safety Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards Operation Before applying power comply with the installation section Additionally the following must be observed Do not remove instrument covers when operating Before the instrument is switched on all protective earth terminals extension cords auto transformers and devices connected to it must be connected to a protective earth via a ground socket Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury Whenever it is likely that the protection has been impaired the instrument must be made inoperative and be secured against any intended operation Make sure that only fuses with the required rated current and of the specified type normal blow time delay and so on are used for replacement The use of repaired fuses and the short circuiting of fuse holders must be avoided Agilent 1260 Infinity RID User Manual 161 12 Appendix 162 Some adjustments described in the manual are made with power supplied to the instrument and protective covers removed Energy available at many points may if contacted result in personal injury Any adjustment maintenance and repair of the opened instrument under voltage should be avoided whenever possible When inevitable this has to be carried out by
45. able disconnected Please contact your Agilent service representative 2 Defective main board Please contact your Agilent service representative 3 Defective heater Please contact your Agilent service representative Agilent 1260 Infinity RID User Manual 107 7 108 Error Information Heater Fuse The electronic fuse of the heater has been activated Probable cause 1 Short in heater circuit 2 Defective main board 3 Defective heater Wrong Temperature Profile Suggested actions Power cycle the detector Please contact your Agilent service representative Please contact your Agilent service representative After turning ON the optical unit heat control the temperature does not increase at a sufficiently fast rate to reach the set point Probable cause 1 Defective main board 2 Defective heater Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Agilent 1260 Infinity RID User Manual Error Information 7 Undecipherable Temperature Signal Probable cause Suggested actions 1 Heater cable disconnected Please contact your Agilent service representative 2 Defective main board Please contact your Agilent service representative 3 Defective heater Please contact your Agilent service representative Maximum Temperature Exceeded The maximum heater temperature has been exceeded Probable cause Suggested actions
46. al Optimizing the Refractive Index Detector 5 7 Use an appropriate response time For most applications a setting of 4 seconds is adequate Only for high speed analyses short columns at high flow rates a lower setting is recommended Bear in mind that even if the response time setting is too high fast peaks will appear a little smaller and broader but retention time and peak areas are still correct and reproducible 8 Recycle mobile phase Use the recycle valve to allow automatic recycling of mobile phase delivered when no analysis is running The pump flow can therefore continue uninterrupted until the next 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 on line vacuum degasser the solvent composition will change When re starting the flow or when using new mobile phase flush each degasser channel used for 10 minutes at the maximum flow rate of the pump with the purge valve of the pump open to avoid a potential over pressure in the RI detector s flow cell 11 Use pre mixed solvents only Don t use a pump for mixing solvents When operating the RI detector together with a qua
47. al detector response if different to be changed to the theoretical value Refractive index calibration is only required after exchange of the optical unit or the main RIM board The Refractive Index Calibration Procedure When Tools required Parts required 118 Recommended after exchange of the optical unit or RIM board Laboratory balance p n Description 1 DAB Ph Eur BP JP NF USP Grade Sucrose 1 9301 1446 Syringe 1 9301 0407 Needle 1 5061 3367 Sample filter 1 0100 1516 Fitting male PEEK 2 pk Agilent 1260 Infinity RID User Manual Test Functions 8 1 Preparation of the sucrose calibration solution a To prepare 25 ml of the calibration solution 87 5 mg of the Sucrose sample is required b Add the weighed amount of sample into a suitable volumetric flask c Dispense 10 ml of LC grade water into the flask and shake or stir to dissolve 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 Using the Agilent LabAdvisor Software B 01 03 SP4 or later there are three screens used for the calibration process a RID Module Service Center via Tools M Generic control parameters m Recycle Valve On Off Recycle Valve on Recycle Valve off m Purge Valve On Off
48. al is zero if the two diodes show the same light level This parameter allows you to store individually the signal measured by the diode 1 Diode 2 signal 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 you to store individually the signal measured by the diode 2 Optical unit temperature This parameter activates the storage of the optical unit temperature signal Polarity This parameter activates the storage of polarity switching during the run Balance signal This parameter activates storage of the diode balance signal during a run This helps to diagnose peaks that exceed the dynamic range of the RID for example in the case of extremely high concentrations signals e Automatic Zero This setting allows you to activate an automatic zeroing of the signal before the run is started If automatic purge is selected the purge will be performed before the automatic zero e Automatic Purge This parameter can be used to do a purge of the reference cell and wait additional time for baseline stabilization It will be initiated each time when the run is started This should only be used if the content of the reference cell is expected to degrade during a run The automatic purge will be finished before the autozero is performed and before the injection is done Agilent 1260 Infinity RID User Manual 71 4 Usi
49. and will improve the performance of the detector Do not overpressurize the flow cell Be aware to not exceed a 5 bar pressure drop after the flow cell when hooking up additional devices like other detectors or a fraction collector If an additional detector is installed place upstream in the flow path it before the G1362A refractive index detector Use the correct solvents To minimize baseline noise and drift solvents must be LC grade and filtered prior to use 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 between pump and column Ensure that the connections from the on line vacuum degasser to the pump and the detector inlet waste and recycle connections are air tight Verify frit filter and fitting quality Partially blocked frits filters and fittings can cause baseline long term noise Verify that the pressure drop across all such parts is within expected limits Control the optical unit temperature Always control the optical unit temperature heater ON for maximum detector sensitivity or with samples that could precipitate in the sample cell at room temperature and set an elevated optical unit temperature at least 5 C above ambient conditions Agilent 1260 Infinity RID User Manu
50. ased on ASTM method E 1303 95 Practice for Refractive 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 Jor Refractive Index Detectors used in Liquid Chromatography measured over 20 minutes Factors that will affect the baseline stability include Variations in the optics or eluent temperature Pressure fluctuations in the sample cell The quality of the water used Air bubbles in the flow cell See Refractive Index Detector Control on page 66 Agilent 1260 Infinity RID User Manual Agilent 1260 Infinity RID User Manual E the Refractive Index Detector 84 Refractive Index Detector Optimization 86 Potential Causes for Baseline Problems Detector Equilibration 87 This chapter provides information on how to optimize the detector Agilent Technologies 83 5 Optimizing the Refractive Index Detector Refractive Index Detector Optimization 84 Follow these thirteen points to optimize the performance of your refractive index detector 1 Position the solvent and waste reservoirs correctly Position the solvent and waste reservoirs above the level of the refractive index detector and solvent pump This maintains a slight pressure in the sample cell
51. ce cycles Initially no EMF limit should be set When instrument performance indicates maintenance is necessary take note of the values displayed by reference liquid age counters Enter these values or a value slightly less than the displayed values as an EMF limit and then reset the EMF counter to zero The next time the EMF counter exceed the new EMF limit the EMF flag will be displayed providing a reminder that maintenance needs to be scheduled Agilent 1260 Infinity RID User Manual 21 1 Introduction to the Refractive Index Detector Instrument Layout 22 The industrial design of the module incorporates several innovative features It uses Agilent s E PAC concept for the packaging of electronics and mechanical assemblies This concept is based upon the use of expanded polypropylene EPP layers foam plastic spacers in which the mechanical and electronic boards components of the module are placed This pack is then housed in a metal inner cabinet which is enclosed by a plastic external cabinet The advantages of this packaging technology are e virtual elimination of fixing screws bolts or ties reducing the number of components and increasing the speed of assembly disassembly e the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations e the plastic layers help cushion the electronic and mechanical parts from physical shock and e the metal inner cabinet sh
52. ce 9 Warnings and Cautions WARNING Toxic flammable and hazardous solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks gt When working with these substances observe appropriate safety procedures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice gt The amount of substances should be reduced to the minimal volume required for the analysis gt Do not operate the instrument in an explosive atmosphere WARNING Electrical shock Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened gt Do not remove the metal top cover of the module No serviceable parts inside gt Only certified persons are authorized to carry out repairs inside the module WARNING Personal injury or damage to the product Agilent is not responsible for any damages caused in whole or in part by improper use of the products unauthorized alterations adjustments or modifications to the products failure to comply with procedures in Agilent product user guides or use of the products in violation of applicable laws rules or regulations gt Use your Agilent products only in the manner described in the Agilent product user guides Agilent 1260 Infinity RID User Manual 131 9 Maintenance
53. damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated condi tions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indi cated conditions are fully under stood and met Agilent 1260 Infinity RID User Manual In This Guide In This Guide This manual covers the Agilent 1260 Infinity Refractive Index Detector G1362A RID 1 Introduction to the Refractive Index Detector This chapter gives an introduction to the Refractive Index Detector 2 Site Requirements and Specifications This chapter provides information on environmental requirements physical and performance specifications 3 Installing the Refractive Index Detector This chapter provides information on unpacking checking on completeness stack considerations and installation of the detector 4 Using the Refractive Index Detector This chapter provides information on how to set up the detector for an analysis and explains the basic settings 5 Optimizing the Refractive Index Detector This chapter provides information on how to optimize the detector 6 Troubleshooting and Diagnostics This chapter gives an overview about the troubleshooting and diagnostic features and the dif
54. dicates dangerous voltages Indicates a protected ground terminal Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in this product The apparatus is marked with this symbol when hot surfaces are available A and the user should not touch it when heated up WARNING aia alerts you to situations that could cause physical injury or death gt Do not proceed beyond a warning until you have fully understood and met the indicated conditions CAUTION A CAUTION alerts you to situations that could cause loss of data or damage of equipment gt Do not proceed beyond a caution until you have fully understood and met the indicated conditions 160 Agilent 1260 Infinity RID User Manual Appendix 12 General Safety Information The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements WARNING Ensure the proper usage of the equipment The protection provided by the equipment may be impaired gt The operator of this instrument is advised to use the equipment in a manner as specified in this manual Safety Standards
55. dition The module is ina not ready state when it is waiting for a specific condition to be reached or completed for example immediately after changing a set point or while a self test procedure is running e An error condition is indicated when the status indicator is red An error condition indicates the module has detected an internal problem which affects correct operation of the module Usually an error condition requires attention e g leak defective internal components An error condition always interrupts the analysis e A red blinking modules with on board LAN or yellow blinking modules without on board LAN indicator indicates that the module is in resident mode e g during update of main firmware A fast red blinking modules with on board LAN or fast yellow blinking modules without on board LAN indicator indicates that the module is in boot loader mode e g during update of main firmware In such a case try to re boot the module or try a cold start Agilent 1260 Infinity RID User Manual 93 6 Troubleshooting and Diagnostics User Interfaces e Depending on the user interface the available tests and the screens reports may vary see Chapter Test Functions and Calibrations e Preferred tool should be the Agilent Diagnostic Software see Agilent Lab Advisor Software on page 95 The Agilent ChemStation B 04 02 and above may not include any maintenance test functions e Screenshots used withi
56. dule to 3396 Integrators p n 03396 60560 Pin 3396 Pin Agilent Signal Name BCD Digit module 1 1 BCD 5 20 ae 2 2 BCD 7 80 K 3 3 BCD 6 40 4 4 BCD4 10 g 5 5 BCDO 1 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 5V Low 154 Agilent 1260 Infinity RID User Manual CAN LAN Cables Identifying Cables 11 Both ends of this cable provide a modular plug to be connected to Agilent modules CAN or LAN connectors CAN Cables p n 5181 1516 5181 1519 LAN Cables p n 5023 0203 5023 0202 Description CAN cable Agilent module to module 0 5 m CAN cable Agilent module to module 1 m Description Cross over network cable shielded 3 m for point to point connection Twisted pair network cable shielded 7 m for point to point connection Agilent 1260 Infinity RID User Manual 155 11 Identifying Cables Agilent Module to PC p n Description G1530 60600 RS 232 cable 2m RS232 61600 RS 232 cable 2 5m Instrument to PC 9 to 9 pin female This cable has special pin out and is not compatible with connecting printers and plotters It s also called Null Modem Cable with full handshaking where the wiring is made between pins 1 1 2 3 3 2 4 6 5 5 6 4 7 8 8 7 9 9 5181 1561 RS 232 cable 8m 156 Agilent 1260 Infinity RID User Manual External Contact Cable 10 lt 6 TG a lt 11 Identifying Cables One end of this cable provides a 15 pin
57. e might be necessary to keep all systems on the same validated revision or if anew module with newer firmware is added to a system or if third part control software requires a special version LAN RS 232 Firmware Update Tool or Agilent Diagnostic Software Instant Pilot G4208A only if supported by module Description 1 Firmware tools and documentation from Agilent web site Read update documentation provided with the Firmware Update Tool To upgrade downgrade the module s firmware carry out the following steps 1 Download the required module firmware the latest LAN RS 232 FW Update Tool and the documentation from the Agilent web http www chem agilent com scripts cag_firmware asp 2 To load the firmware into the module follow the instructions in the documentation Module Specific Information There is no specific information for this module Agilent 1260 Infinity RID User Manual Maintenance 9 Replacing the Interface Board When For all repairs inside the detector or for installation of the board Parts required p n Description 1 G1351 68701 Interface board BCD with external contacts and BCD outputs 1 G1369B or Interface board LAN G1369 60002 Setting the 8 bit Configuration Switch without On Board LAN on page 33 1 To replace the interface board unscrew the two screws remove the board slide in the new interface board and fix it with the board s screws Interface board
58. e relying on operation of others 7 READY H System is ready for next analysis Receiver is any sequence controller 8 STOP L Request to reach system ready state as soon as possible for example stop run abort or finish and stop injection Receiver is any module performing run time controlled activities 9 START REQUEST L Request to start injection cycle for example by start key on any module Receiver is the autosampler Special Interfaces Some modules have module specific interfaces connectors They are described in the module documentation 30 Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 Setting the 8 bit Configuration Switch On Board LAN The 8 bit configuration switch is located at the rear of the module Switch settings provide configuration parameters for LAN serial communication protocol and instrument specific initialization procedures All modules with on board LAN e g G1315 65C D G1314D E F G4212A B G4220A e Default is ALL switches DOWN best settings Bootp mode for LAN e For specific LAN modes switches 3 8 must be set as required For boot test modes switches 1 2 must be UP plus required mode f S oe Figure 11 Location of Configuration Switch example shows a G4212A DAD To perform any LAN configuration SW1 and SW2 must be set to OFF For details on the LAN settings configuration refer to chapter LAN Configurati
59. ect the LAN connection to the LAN interface board in the detector 7 Connect the analog cable optional for a chart recorder integrator or other data collection device 8 Connect the APG remote cable optional for non Agilent modules Agilent 1260 Infinity RID User Manual 57 3 Installing the Refractive Index Detector Installing the Detector 9 Turn ON power by pushing the button at the lower left hand side of the detector The status LED should be green APG remote Analog signal va zo bar 5000 Configuration Steele eres j eje mabe i sere Security lever Figure 21 Rear View of Detector NOTE The GPIB interface has been removed with the introduction of the Agilent 1260 Infinity modules 58 Agilent 1260 Infinity RID User Manual Installing the Refractive Index Detector 3 Flow Connections Tools required Parts required Hardware required Preparations Y inch wrench p n Description 1 G1362 68706 Interface tubing kit 1 G1362 87300 Interfacing capillary Other modules Detector is installed in the LC system WARNING Toxic flammable and hazardous solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks gt When working with these substances observe appropriate safety procedures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data shee
60. electing the setting which you want to use for RS 232C communication The number 0 means that the switch is down and 1 means that the switch is up Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 Table7 Baudrate Settings without on board LAN Switches Baud Rate Switches Baud Rate 3 4 5 3 4 5 0 0 0 9600 1 0 0 9600 0 0 1 1200 1 0 1 14400 0 1 0 2400 1 1 0 19200 0 1 1 4800 1 1 1 38400 Table 8 Data Bit Settings without on board LAN Switch 6 Data Word Size 0 7 Bit Communication 1 8 Bit Communication Table9 Parity Settings without on board LAN Switches Parity 7 e 0 0 No Parity 1 0 Odd Parity 1 1 Even Parity One start bit and one stop bit are always used not selectable Per default the module will turn into 19200 baud 8 data bit with no parity Agilent 1260 Infinity RID User Manual 35 1 Introduction to the Refractive Index Detector Special Settings The special settings are required for specific actions normally in a service case The tables include both settings for modules with on board LAN and without on board LAN They are identified as LAN and no LAN Boot Resident Firmware update procedures may require this mode in case of firmware loading errors main firmware part If you use the following switch settings and power the instrument up again the instrument firmware stays in the resident mode It is not o
61. er Manual 7 Error Information What Are Error Messages 99 General Error Messages 100 Timeout 100 Shut Down 101 Remote Timeout 101 Synchronization Lost 102 Leak 102 Leak Sensor Open 103 Leak Sensor Short 103 Compensation Sensor Open 104 Compensation Sensor Short 104 Fan Failed 105 OpenCover 105 Cover Violation 106 Refractive Index Detector Specific Error Messages 107 Thermal Fuse Open 107 Heater Resistance Too High 107 Heater Fuse 108 Wrong Temperature Profile 108 Undecipherable Temperature Signal 109 Maximum Temperature Exceeded 109 Purge Valve Fuse Blown 110 Recycle Valve Fuse Blown 110 Purge Valve Not Connected 111 Recycle Valve Missing 111 Lamp Voltage tooLow 112 Lamp Voltage too High 112 Lamp Current too High 112 ae Agilent Technologies 97 7 Error Information Lamp Current too Low 113 Wait Function Timed Out 113 Not Ready Messages 114 Purge Time Running 114 Wait for Purge 114 Unbalanced Diodes 115 Not Enough Light 115 Too Much Light 115 This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions 98 Agilent 1260 Infinity RID User Manual Error Information 7 What Are Error Messages Error messages are displayed in the user interface when an electronic mechanical or hydraulic flow path failure occurs which requires attention before the analysis can be continued for example repair or exchange of consu
62. error message is generated Probable cause Suggested actions 1 Leak sensor not connected to the main Please contact your Agilent service board representative 2 Defective leak sensor Please contact your Agilent service representative 3 Leak sensor incorrectly routed being Please contact your Agilent service pinched by a metal component representative Leak Sensor Short The leak sensor in the module has failed short circuit The current through the leak sensor is dependent on temperature A leak is detected when solvent cools the leak sensor causing the leak sensor current to change within defined limits If the current increases above the upper limit the error message is generated Probable cause Suggested actions 1 Defective flow sensor Please contact your Agilent service representative Agilent 1260 Infinity RID User Manual 103 7 104 Error Information Compensation Sensor Open The ambient compensation sensor NTC on the main board in the module has failed open circuit The resistance across the temperature compensation sensor NTC on the main board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor increases above the upper limit the error message is generated Probable cause Suggested actions 1 Defective main board Please contact your Agilent service representative Compensation
63. ervice office Table 14 Delivery Checklist 1260 RID Description Quantity Detector 1 Power cable 1 User Manual on User Documentation CD 1 Accessory kit p n G1362 68755 1 Agilent 1260 Infinity RID User Manual Installing the Refractive Index Detector 3 Jnpacking the Det Accessory Kit Accessory kit p n G1362 68755 contains some accessories needed for the installation of the detector p n Description G1362 68706 Interface tubing kit G1362 87300 Interfacing capillary G1362 87301 Restriction capillary 5181 1516 CAN cable Agilent module to module 0 5 m 0100 1847 PEEK adapter 1 4 28 to 10 32 Adapter AIV to solvent inlet tubes a ee BE e rmen e aan A e Figure 13 Interface Tubing Kit Parts ST 1 S Figure 14 Interfacing Capillary Parts Agilent 1260 Infinity RID User Manual 49 3 Installing the Refractive Index Detector Unpacking the Detector Figure 15 Restriction Capillary Parts 50 Agilent 1260 Infinity RID User Manual Installing the Refractive Index Detector 3 Optimizing the Stack Configuration If your detector is part of a complete Agilent 1200 Infinity Series system you can ensure optimum performance by installing the following configuration This configuration optimizes the system flow path ensuring minimum delay volume Agilent 1260 Infinity RID User Manual 51 3 Installing the Refractive Index Detector Optimizing the Stack Configuration Optimizing the One Stack Confi
64. f the instrument can be easily reached and unplugged gt Provide sufficient space behind the power socket of the instrument to unplug the cable 40 Agilent 1260 Infinity RID User Manual Site Requirements and Specifications 2 Power Cords Different power cords are offered as options with the module The female end of all power cords is identical It plugs into the power input socket at the rear The male end of each power cord is different and designed to match the wall socket of a particular country or region Absence of ground connection or use of unspecified power cord The absence of ground connection or the use of unspecified power cord can lead to electric shock or short circuit gt Never operate your instrumentation from a power outlet that has no ground connection gt Never use a power cord other than the Agilent Technologies power cord designed for your region Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury gt Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Unintended use of supplied power cords Using power cords for unintended purposes can lead to personal injury or damage of electronic equipment gt Never use the power cords that Agilent Technologies supplies with this instrument for any other equi
65. ferent user interfaces 7 Error Information This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions Agilent 1260 Infinity RID User Manual In This Guide 8 Test Functions This chapter describes the detector s built in test functions 9 Maintenance This chapter provides general information on maintenance of the detector 10 Parts for Maintenance This chapter provides information on parts for maintenance 11 Identifying Cables This chapter provides information on cables used with the Agilent 1260 Infinity LC modules 12 Appendix This chapter provides safetey and other general information 4 Agilent 1260 Infinity RID User Manual Contents Contents Introduction to the Refractive Index Detector 9 Introduction to the Refractive Index Detector 10 How the Detector Operates 11 Detection Principle 13 Flow Path 16 Early Maintenance Feedback 21 Instrument Layout 22 Electrical Connections 23 Interfaces 25 Setting the 8 bit Configuration Switch On Board LAN 31 Site Requirements and Specifications 39 Site Requirements 40 Physical Specifications 43 Performance Specifications 44 Installing the Refractive Index Detector 47 Unpacking the Detector 48 Optimizing the Stack Configuration 51 Installing the Detector 56 Flow Connections 59 Using the Refractive Index Detector 63 Operation of the Refract
66. g a Checkout Sample 72 Checking Baseline Noise and Drift 76 Setting the Test Conditions 76 Evaluation 82 This chapter provides information on how to set up the detector for an analysis and explains the basic settings ot Agilent Technologies 63 4 Using the Refractive Index Detector Operation of the Refractive Index Detector This chapter can be used for e preparing the system e to learn the set up of an HPLC analysis and e 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 e Learn about special settings Before Using the System Solvent Information Consult the manual of your pump about suitable solvents Priming and Purging the System When the solvents have been exchanged or the pumping system has been turned off for a certain time for example overnight oxygen will re diffuse into the solvent channel between the solvent reservoir vacuum degasser when available in the system and the pump Solvents containing volatile ingredients will slightly lose these Therefore priming of the pumping system is required before starting an application 64 Agilent 1260 Infinity RID User Manual Using the Refractive Index Detector 4 Table 15 Choice of Priming Solvents for Different Purposes Activity Solvent Comments After an installation lsopropanol Best solvent to flush air out of the system When switchin
67. g between reverse lsopropanol Best solvent to flush air out of the phase and normal phase both times system After an installation Ethanol or Methanol Alternative to Isopropanol second choice if no Isopropanol is available To clean the system when using Bidistilled water Best solvent to re dissolve buffer buffers crystals After a solvent change Bidistilled water Best solvent to re dissolve buffer crystals After the installation of normal phase Hexane 5 Isopropanol Good wetting properties seals P N 0905 1420 1 Open the purge valve of your pump by turning it counterclockwise and set flow rate to 3 5 ml min 2 Flush all tubes with at least 30 ml of solvent 3 Set flow to required value of your application and close the purge valve Pump for approximately 30 minutes before starting your application for some solvents an even longer flush and equilibration time might be needed Agilent 1260 Infinity RID User Manual 65 4 66 Using the Refractive Index Detector Refractive Index Detector Control The following operating instructions were generated using the Agilent B 01 03 ChemStation as operating software How To Get There The RID Control dialog box is displayed when you select More RID from the Instrument menu More RID is available in Full Menus only and select Control from the More RID submenu RID Control Instrument 1 q x m Heater on off Recycling Yalve m Error
68. guration Solvent cabinet Vacuum degasser Instant pilot Autosampler Column compartment Detector Figure 16 Recommended Stack Configuration Front View 52 Agilent 1260 Infinity RID User Manual Installing the Refractive Index Detector 3 Optimizing the Stack Configuration IMU NMI Remote cable Analog signal pump pressure CAN Bus cable AC power CAN Bus cable LAN to control software requires Interface card G1369B Analog signal detector AC power Figure 17 Recommended Stack Configuration Rear View Agilent 1260 Infinity RID User Manual 53 3 Installing the Refractive Index Detector Optimizing the Two Stack Configuration To avoid excessive height of the stack when the autosampler thermostat is added to the system it is recommended to form two stacks Some users prefer the lower height of this arrangement even without the autosampler thermostat A slightly longer capillary is required between the pump and autosampler See Figure 18 on page 54 and Figure 19 on page 55 Instant Pilot Detector Column compartment
69. he Agilent 1260 Infinity LC modules ot Agilent Technologies 145 11 Identifying Cables Cable Overview 146 Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Analog cables p n Description 35900 60750 Agilent module to 3394 6 integrators 35900 60750 Agilent 35900A A D converter 01046 60105 Analog cable BNC to general purpose spade lugs Remote cables p n Description 03394 60600 Agilent module to 3396A Series integrators 3396 Series II 3395A integrator see details in section Remote Cables on page 150 03396 61010 Agilent module to 3396 Series III 3395B integrators 5061 3378 Agilent module to Agilent 35900 A D converters or HP 1050 1046A 1049A 01046 60201 Agilent module to general purpose BCD cables p n Description 03396 60560 Agilent module to 3396 integrators G1351 81600 Agilent module to general purpose Agilent 1260 Infinity RID User Manual CAN cables p n 5181 1516 5181 1519 LAN cables p n 5023 0203 5023 0202 RS 232 cables p n G1530 60600 RS232 61600 5181 1561 Identifying Cables 11 Description CAN cable Agilent module to module 0 5 m CAN cable Agilent module to module 1 m Description Cross over network cable shielded 3 m for point to point connection Twisted pair network cable shielded 7 m for point to point connection Description RS 232 cable
70. ields the internal electronics from electromagnetic interference and also helps to reduce or eliminate radio frequency emissions from the instrument itself Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 Electrical Connections The CAN bus is a serial bus with high speed data transfer The two connectors for the CAN bus are used for internal module data transfer and synchronization e One analog output provides signals for integrators or data handling systems The interface board slot is used for external contacts and BCD bottle number output or LAN connections The REMOTE connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features such as start stop common shut down prepare and so on e With the appropriate software the RS 232C connector may be used to control the module from a computer through a RS 232C connection This connector is activated and can be configured with the configuration switch e The power input socket accepts a line voltage of 100 240 VAC 10 witha line frequency of 50 or 60 Hz Maximum power consumption varies by module There is no voltage selector on your module because the power supply has wide ranging capability There are no externally accessible fuses because automatic electronic fuses are implemented in the power supply Never use cables other than the ones supplied by Agilent Technol
71. ilt up algae Therefore do not leave aqueous solvents sitting in the flow cell Add a small of organic solvents e g acetonitrile or methanol 5 Use of Solvents Observe the following recommendations on the use of solvents e Brown glass ware can avoid growth of algae e Small particles can permanently block capillaries and valves Therefore always filter solvents through 0 4 um filters e Avoid the use of the following steel corrosive solvents Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like sulfuric acid and nitric acid especially at higher temperatures if your chromatography method allows replace by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2CHCl Oo 2COCly 2HCI This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol Agilent 1260 Infinity RID User Manual 167 12 Appendix Chromatographic grade ethers which can contain peroxides for example THF dioxane di isopropylether such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides Solvents containing strong complexing agents e g EDTA Mixtures of carbon tetrachloride with 2 propanol or TH
72. ing diodes to generate a refractive used to ensure that it is free of air bubbles or index signal other contamination Too Much Light The amount of light falling on the light receiving diodes is too high to generate a refractive index signal Probable cause Suggested actions 1 The sample cell content is varying too much Purge reference and sample cell from the reference cell Agilent 1260 Infinity RID User Manual 115 7 Error Information Not Ready Messages 116 Agilent 1260 Infinity RID User Manual j Agilent 1260 Infinity RID User Manual ee 8 Test Functions e E e j Refractive Index Calibration 118 Optical Balance 123 Using the Build in Test Chromatogram 126 Procedure Using the Agilent LabAdvisor 126 This chapter describes the detector s built in test functions Agg Agilent Technologies 117 8 Test Functions Refractive Index Calibration Refractive Index Calibration The refractive index calibration is based on a sucrose calibration solution which has a known refractive index compared to LC grade water After both the sample and reference 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 actu
73. irective 2002 96 EC marking requirements The affixed label indicates that you must not discard this electrical electronic product in domestic household waste Product Category With reference to the equipment types in the WEEE Directive Annex I this product is classed as a Monitoring and Control instrumentation product Do not dispose off in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com for more information Agilent 1260 Infinity RID User Manual 163 12 Appendix Lithium Batteries Information Lithium batteries may not be disposed off into the domestic waste Transportation of discharged Lithium batteries through carriers regulated by IATA ICAO ADR RID IMDG is not allowed Danger of explosion if battery is incorrectly replaced gt Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries gt Replace only with the same or equivalent type recommended by the equipment manufacturer Lithiumbatteri Eksplosionsfare ved fejlagtig handtering Udskiftning ma kun ske med batteri af samme fabrikat og type gt Lever det brugte batteri tilbage til leverand ren Lithiumbatteri Eksplosionsfare Ved udskiftning benyttes kun batteri som anbefalt av apparatfabrikanten gt Brukt batteri returneres appararleverandoren 164 Bij dit apparaat zijn batterijen geleverd Wanneer de
74. ission 166 Solvent Information 167 Agilent Technologies on Internet 169 Agilent 1260 Infinity RID User Manual Contents 8 Agilent 1260 Infinity RID User Manual Agilent 1260 Infinity RID User Manual 1 Introduction to the Refractive Index Detector Introduction to the Refractive Index Detector 10 How the Detector Operates 11 Detection Principle 13 Flow Path 16 Early Maintenance Feedback 21 EMF Counters 21 Using the EMF Counters 21 Instrument Layout 22 Electrical Connections 23 Rear View of the Module 24 Serial Number Information 24 Interfaces 25 Overview Interfaces 27 Setting the 8 bit Configuration Switch On Board LAN 31 Communication Settings for RS 232C 34 Special Settings 36 This chapter gives an introduction to the Refractive Index Detector ee Agilent Technologies 1 Introduction to the Refractive Index Detector Introduction to the Refractive Index Detector 10 The detector is designed for highest optical performance GLP compliance and easy maintenance It includes the following features advanced temperature controlled detector 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 40 000 hours automatic light intensity control circuit to ensure the optimum performance of the optics integrated diagnostics for efficient troub
75. its baseline Therefore the detector will trace down any instabilities in the system and the environment as well It may sometimes appear as if the detector itself was unstable or generating an unstable baseline where in fact the detector is simply displaying the instabilities of the environment and the rest of the system By this 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 the better the longer the system is used under identical and stable conditions Keep the temperature in your laboratory and system constant and controlled Ideally a system with an RID should be used always with the same type of analysis stable solvent composition temperature flow rates don t switch the pump off after analysis instead just recycle solvents or at least reduce only the flow Switch valves and settings only when needed Don t expose the detector to draft of air or to vibrations A change of any of these parameters may require a considerable amount of time for re equilibration Agilent 1260 Infinity RID User Manual 87 5 Optimizing the Refractive Index Detector Refractive Index Detector Optimization
76. ive Index Detector 64 Running a Checkout Sample 72 Checking Baseline Noise and Drift 76 Optimizing the Refractive Index Detector 83 Refractive Index Detector Optimization 84 Agilent 1260 Infinity RID User Manual Contents Troubleshooting and Diagnostics 89 Overview of the Module s Indicators and Test Functions 90 Status Indicators 92 User Interfaces 94 Agilent Lab Advisor Software 95 Error Information 97 What Are Error Messages 99 General Error Messages 100 Refractive Index Detector Specific Error Messages 107 Not Ready Messages 114 Test Functions 117 Refractive Index Calibration 118 Optical Balance 123 Using the Build in Test Chromatogram 126 Maintenance 129 Introduction to Maintenance 130 Warnings and Cautions 131 Detector Maintenance Procedures 133 Cleaning the Module 134 Flow Cell Flushing 135 Correcting Leaks 136 Replacing Leak Handling System Parts 137 Replacing the Detector s Firmware 138 Replacing the Interface Board 139 10 Parts for Maintenance 141 Accessory Kits 142 Agilent 1260 Infinity RID User Manual Contents 11 Identifying Cables 145 Cable Overview 146 Analog Cables 148 Remote Cables 150 BCD Cables 153 CAN LAN Cables 155 Agilent Module to PC 156 External Contact Cable 157 12 Appendix 159 General Safety Information 160 The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC 163 Lithium Batteries Information 164 Radio Interference 165 Sound Em
77. l contact cable 15 7 F fan failed 105 features Agilent 1260 Infinity RID User Manual instrument layout 22 safety and maintenance 45 firmware updates 138 138 upgade downgrade 138 upgrade downgrade 138 flow cell pressure 84 flow cell flushing 135 solvent information 167 flow cell 167 flow path 16 frequency range 43 frits and filters 84 front view of module 56 G general error messages 100 GLP features 45 GLP 10 how the detector operates 11 how the detector operates automatic purge 16 automatic recycling after analysis 16 automatic zero before analysis 16 flow path 16 recycle valve 16 how the detector operates purge valve 16 humidity 43 installation bench space 42 delivery checklist 48 environment 42 42 42 flow connections 59 of in waste and recycle capillaries 59 ofthe detector 56 site requirements 39 unpacking 48 interface board BCD LAN replacing 139 interfaces 25 internet 169 introduction introduction to the detector 10 operation of the detector 11 L LAN cable 155 leak handling system replacing 137 leak sensor open 103 leak sensor short 103 leak 102 leaks correcting 136 light intensity control 10 line frequency 43 line voltage 43 lithium batteries 164 M maintenance definition of 130 replacing firmware 138 138 measurements 14 message cover violation 106 heater fuse 108 heater resistance too high 107 ignition without cover 105 105 lamp current too high 112 171
78. lect Setup RID signal from the Instrument menu The More button displays additional Menus x optical Unit Temperature r Time Analog Output 4 0 4 YE Stoptime Zero Offset as Pump 4 mi 20 00 d min a r Polarity A a Posttime Attenuation positive x ot gt min s00 10 3 gt naw negative Automatic recycling r Peakwidth Responsetime mStore additionally after analysis eo off p gt 0 2 min 4 s standare pa I Diode 1 Signal I Diode 2 Signal r Limetable J Optical Unit Temperature Line Time Polarity Peakwidth inser J Polarity Append J Balance Signal m Automatic zero before analysis on C off Automatic purge gt purgetime 0 00 min Canal Help More waittime 0 00 min Figure 24 More RID Settings Analog Output If the Analog Output is used a zero offset limits between 1 and 99 can be selected to enable the display of negative peaks The attenuation settings helps to keep all peaks on scale Choose the appropriate setting from the list Store Additionally Here you can choose to store additional signal that may help during method development and diagnosis with the RID The following parameters can be selected 70 Agilent 1260 Infinity RID User Manual Using the Refractive Index Detector 4 Diode 1 signal The RID signal is based on the ratio of the light level that is measured by two photodiodes The RID sign
79. leshooting built in refractive index calibration front access to valves and capillaries for easy maintenance For specifications see Performance Specifications on page 44 Figure 1 The Agilent 1260 Infinity Refractive Index Detector Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 How the Detector Operates Refractive index When a beam of light passes from one medium into another the wave 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 5 eis n sina Where n Refractive index of medium 1 relative to medium 2 ns Refractive index of medium 2 n Refractive index of medium 1 ay angle of incident light in medium 1 angle of refraction in medium 2 Medium 1 Medium 2 Figure 2 Light Refraction Agilent 1260 Infinity RID User Manual 11 1 12 Introduction to the Refractive Index Detector According to the formula below small angles of external deflection are proportional to the difference between the refractive indices of medium 1 and medium 2 ny 12 tan y Fa Where e y angle of external deflection ny Refractive index of medium 2 n Refractive index of medium 1 Factors that Affect Refractive Index The refractive index of a medium is affected by a number of factor
80. ll in the case of solvent change or reference cell contamination Enter a time interval minutes to purge the reference cell of the Agilent 1260 Infinity RID This will be started immediately if you click OK on this window Allow additional time for baseline stabilization after purging At Power On When activated the optical unit heater is turned on automatically when the RID is switched on For shortest equilibration times Agilent recommends to leave this function always on 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 Select Turn Heater on at to activate the date and time fields and enter the date and time in the appropriate fields in the specified format Agilent 1260 Infinity RID User Manual 67 4 Using the Refractive Index Detector Refractive Index Detector Settings The following operating instructions were generated using the Agilent B 01 03 ChemStation as operating software How To Get There The Agilent 1260 Infinity RID Signal dialog box is displayed when you select Setup RID Signal from the Instrument menu RID signal Instrumenta S optical Unit Temperature m Time 3940 4 Cc Stoptime as Pump 4 mi 20 00 3 min r Polarity f P Posttime positive olt 4 A min C negative gt Automatic recycling r Peakwidth Responsetime after analysis ia off p gt
81. mables is necessary In the event of such a failure the red status indicator at the front of the module is switched on and an entry is written into the module logbook Agilent 1260 Infinity RID User Manual 99 7 Error Information General Error Messages General error messages are generic to all Agilent series HPLC modules and may show up on other modules as well Timeout The timeout threshold was exceeded Probable cause Suggested actions 1 The analysis was completed successfully Check the logbook for the occurrence and and the timeout function switched off the source of a not ready condition Restart the module as requested analysis where required 2 Anot ready condition was present duringa Check the logbook for the occurrence and sequence or multiple injection run for a source of a not ready condition Restart the period longer than the timeout threshold analysis where required 100 Agilent 1260 Infinity RID User Manual Shut Down Error Information 7 An external instrument has generated a shut down signal on the remote line The module continually monitors the remote input connectors for status signals A LOW signal input on pin 4 of the remote connector generates the error message Probable cause 1 Leak detected in an external instrument with a remote connection to the system 2 Shut down in an external instrument with a remote connection to the system 3 The degasser failed to generate sufficient vacuum
82. mp is illuminated The detector is turned off when the line power switch is protruding and the green light is OFF Module is partially energized when switched off as long as the power cord is plugged in Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened and the module is connected to power gt Make sure that it is always possible to access the power plug gt Remove the power cable from the instrument before opening the cover gt Do not connect the power cable to the Instrument while the covers are removed 56 The detector was shipped with default configuration settings To change these settings see Setting the 8 bit Configuration Switch without On Board LAN on page 33 1 Install the LAN interface board in the detector if required see Replacing the Interface Board on page 139 2 Place the detector in the stack or on the bench in a horizontal position Agilent 1260 Infinity RID User Manual Installing the Refractive Index Detector 3 Installing the D 3 Ensure the line power switch at the front of the detector is OFF green yellow red ies gt Line power switch with green light d Figure 20 Front View of Detector 4 Connect the power cable to the power connector at the rear of the detector Connect the CAN cable to other Agilent modules 6 Ifan Agilent ChemStation is the controller conn
83. n these procedures are based on the Agilent Lab Advisor Software 94 Agilent 1260 Infinity RID User Manual Troubleshooting and Diagnostics 6 Agilent Lab Advisor Software The Agilent Lab Advisor software is a standalone product that can be used with or without data system Agilent Lab Advisor software helps to manage the lab for high quality chromatographic results and can monitor in real time a single Agilent LC or all the Agilent GCs and LCs configured on the lab intranet Agilent Lab Advisor software provides diagnostic capabilities for all Agilent 1200 Infinity Series modules This includes diagnostic capabilities calibration procedures and maintenance routines for all the maintenance routines The Agilent Lab Advisor software also allows users to monitor the status of their LC instruments The Early Maintenance Feedback EMF feature helps to carry out preventive maintenance In addition users can generate a status report for each individual LC instrument The tests and diagnostic features as provided by the Agilent Lab Advisor software may differ from the descriptions in this manual For details refer to the Agilent Lab Advisor software help files This manual provides lists with the names of Error Messages Not Ready messages and other common issues Agilent 1260 Infinity RID User Manual 95 6 Troubleshooting and Diagnostics Agilent Lab Advisor Software 96 Agilent 1260 Infinity RID User Manual Agilent 1260 Infinity RID Us
84. nected to Agilent Module to 3396A Integrators p n 03394 60600 Pin 3394 Pin Agilent Signal Name Active module TTL E 9 1 White Digital ground NC 2 Brown Prepare run Low 80 7 3 3 Gray Start Low x 3 NC 4 Blue Shut down Low e o gt NC 5 Pink Not connected le NC 6 Yellow Power on High 5 14 7 Red Ready High 1 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent Module to 3396 Series II 3395A Integrators Use the cable Agilent module to 3396A Series I integrators p n 03394 60600 and cut pin 5 on the integrator side Otherwise the integrator prints START not ready Agilent 1260 Infinity RID User Manual Identifying Cables 11 Agilent Module to 3396 Series III 3395B Integrators p n 03396 61010 Pin 33XX Pin Agilent Signal Name Active module TTL 9 1 White Digital ground NC 2 Brown Prepare run Low 80 A 3 3 Gray Start Low A NC 4 Blue Shut down Low e o NC 5 Pink Not connected le NC 6 Yellow Power on High 14 7 Red Ready High 4 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent Module to Agilent 35900 A D Converters p n 5061 3378 Pin 35900 A D Pin Agilent Signal Name Active module TTL 1 White 1 White Digital ground 2 Brown 2 Brown Prepare run Low 3 Gray 3 Gray Start Low 4 Blue 4 Blue Shut down Low
85. ng When Tools required Parts required If flow cell is contaminated Glass syringe adapter Description 1 Strong solvent tubings to waste Dangerous solvents The strong solvents used in this procedure are toxic and flammable and proper precautions are necessary gt Wear protective gloves and goggles gt Don t expose yourself to the vapors Aqueous solvents in the flow cell can build up algae Therefore do not leave aqueous solvents in the flow cell for long periods Add a small percentage of organic solvents e g Acetonitrile or Methanol 5 The strong solvent should dissolve any potential contaminants in the flow cell For example water for aqueous mobile phase buffers chloroform or tetrahydrofuran for not water soluble contaminants In case the cell is contaminated follow the procedure below 1 Flush with the strong solvent 2 Leave this solution in the cell for about one hour 3 Flush with mobile phase Do not exceed the flow cell pressure limit of 5 bar 0 5 MPa Agilent 1260 Infinity RID User Manual 135 9 Maintenance Correcting Leaks Correcting Leaks When If a leakage has occurred in the valve area or at the capillary connections Tools required Tissue Two 1 4 inch wrenches for capillary connections 1 Remove the front cover 2 Open the service door 3 Use tissue to dry the leak sensor area and the leak pan 4 Observe the interface ports and the valve area for leaks and correct if
86. ng the Refractive Index Detector Running a Checkout Sample When Parts required 72 This chapter describes the check out of the Agilent 1260 Infinity Refractive Index Detector using the Agilent isocratic checkout sample If you want to checkout the detector p n Description 1 993967 902 Zorbax Eclipse XDB C18 150mm x 4 6mm i d 1 01080 68704 Agilent isocratic checkout sample 1 Turn the detector on You are now ready to change the settings of your detector 2 Set up the instrument with the following chromatographic conditions Table 16 Chromatographic Conditions Mobile phases 30 Water 70 Acetonitrile Column Zorbax Eclipse XDB C18 150 mm x 4 6 mm i d Sample Isocratic standard sample Flow rate 1 5 ml min Stroke A 20 pl Stop time 10 min Injection volume 20 pl Column compartment temperature 25 C Optical unit Temperature 35 C Polarity Positive Peak Width Response time 0 2 min 4 s standard Agilent 1260 Infinity RID User Manual Using the Refractive Index Detector 4 Running a Checkout Sample 3 Set the RID setpoints according to Figure 25 on page 73 RID Signal Instrument O Figure 25 RID Check Out Sample Parameters Agilent 1260 Infinity RID User Manual 73 4 Using the Refractive Index Detector Running a Checkout Sample 4 Turn the heater ON and purge the detector reference cell for 20 minutes as shown in Figure 26 on page 74 RID Control Instrument 2 Figure 26 RID
87. nt 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 indication for a general system or environmental instability system or laboratory might not be thermally stable control instrument and laboratory temperature Verify that the solvent properties are constant over time flush out contamination use only stabilized and premixed solvents Clean the parts in the flow path and allow the system to be flushed out and equilibrated Drift Excessive drift is an indication for a general system or environmental instability system or laboratory might not be thermally stable control instrument and laboratory temperature Verify that the solvent properties are constant over time flush out of contamination use only stabilized solvents Clean parts in the flow path and allow the system to be flushed out and equilibrated Agilent 1260 Infinity RID User Manual Optimizing the Refractive Index Detector 5 Detector Equilibration The Refractive Index RI is a function of temperature pressure and a property of the used solvent it changes with solvent composition degassing level and due to any trace of contamination Therefore the Refractive Index Detector will detect any change in any of these parameters as a change in its signal and a variation of
88. ogies to ensure proper functionality and compliance with safety or EMC regulations Agilent 1260 Infinity RID User Manual 23 1 Introduction to the Refractive Index Detector Electrical Connections Rear View of the Module Figure 9 Rear View of Detector Electrical Connections and Label NOTE The GPIB interface has been removed with the introduction of the 1260 Infinity modules 24 Serial Number Information The serial number information on the instrument labels provide the following information CCXZZ00000 Format CC Country of manufacturing DE Germany X Alphabetic character A Z used by manufacturing ZZ Alpha numeric code 0 9 A Z where each combination unambiguously denotes a module there can be more than one code for the same module 00000 Serial number Agilent 1260 Infinity RID User Manual Interfaces Introduction to the Refractive Index Detector 1 The Agilent 1200 Infinity Series modules provide the following interfaces Table 1 Agilent 1200 Infinity Series Interfaces Module CAN LAN BCD optional LAN on board RS 232 Analog APG Special Remote Pumps G1310B Iso Pump 2 Yes G1311B Quat Pump G1311C Quat Pump VL G1312B Bin Pump G1312C Bin Pump VL 1376A Cap Pump G2226A Nano Pump G4220A B Bin Pump 2 No G1361A Prep Pump 2 Yes Samplers G1329B ALS 2 Yes G2260A Prep ALS G1364B FC PS 2 Yes G1364C FC AS
89. on Agilent 1260 Infinity RID User Manual 31 1 Introduction to the Refractive Index Detector Table 4 8 bit Configuration Switch with on board LAN Mode Function SW 1 SW 2 SW 3 SW 4 SW 5 SW 6 SW7 SW 8 LAN 0 0 Link Configuration Init Mode Selection Auto negotiation 0 x x x x X 10 MBit half duplex 1 0 0 X x xX 10 MBit full duplex 1 0 1 Xx x xX 100 MBit half duplex 1 1 0 X X X 100 MBit full duplex 1 1 1 x xX xX Bootp x x Xx 0 0 0 Bootp amp Store x xX x 0 0 1 Using Stored x X x 0 1 0 Using Default x X x 0 1 1 TEST 1 1 System NVRAM Boot Resident System 1 X Revert to Default Data Coldstart x x x 1 Legend 0 switch down 1 switch up x any position When selecting the mode TEST the LAN settings are Auto Negotiation amp Using Stored For explanation of Boot Resident System and Revert to Default Data Coldstart refer to Special Settings on page 36 32 Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 Setting the 8 bit Configuration Switch without On Board LAN The 8 bit configuration switch is located at the rear of the module Modules that do not have their own LAN interface e g the TCC can be controlled through the LAN interface of another module and a CAN connection to that module Figure 12 Configuration switch settings depend on configured mode All modules without on board LAN e default is ALL DIPS DOWN best settings
90. ons and warnings 131 check out sample setting the chromatographic conditions 72 checking baseline noise and drift setting the test conditions 76 checking baseline noise and drift evaluation 82 cleaning 134 Communication settings RS 232C 34 compensation sensor open 104 compensation sensor short 104 compliance 10 condensation 42 configuration stack 51 two stack 54 control 66 D defect on arrival 48 degasser 85 delivery checklist 48 detection principle 13 detector design 13 Diagnostic software 95 dimensions 43 drift 86 E early maintenance feedback EMF 21 electrical connections descriptions of 23 Agilent 1260 Infinity RID User Manual Index EMF early maintenance feedback 21 time since last purge 21 42 42 42 equilibration 87 error messages fan failed 105 error messages compensation sensor open 104 compensation sensor short 104 cover violation 106 heater fuse 108 heater resistance too high 107 ignition without cover 105 105 amp currenttoolow 113 amp current too high 112 amp voltage toolow 112 amp voltage too high 112 eak sensor open 103 eak sensor short 103 eak 102 maximum temperature exceeded 109 purge valve fuse blown 110 purge valve not connected 111 recycle valve fuse blown 110 recycle valve missing 111 remote timeout 101 shut down 101 synchronization lost 102 thermal fuse open 107 timeout 100 undecipherable temperature signal 109 wrong temperature profile 108 environment externa
91. or Sample cell Slit Figure 3 Detection Principle Measurements Initially both sample and reference cell are flushed with mobile phase The reference cell is then closed and solvent flows only through the sample cell The refractive index of the mobile phase in both cells is the same and the position of the zero glass can be adjusted so that the detector is in optical balance with an equal amount of light falls on each diode When sample 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 Refractive Index Units nRIU corresponds to the difference between the refractive index of sample in the sample cell and the mobile phase in the reference cell Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 Detection Principle Lamp Condenser lens Incident light Diodes Zero glass Deflected light Collimator lens Sample cell Reference cell Mirror Figure 4 Optical Path Agilent 1260 Infinity RID User Manual 15 1 Introduction to the Refractive Index Detector Flow Path 16 The column eluent enters the optical unit through the in p
92. ort and passes through a heat exchanger The combination of the heat exchanger and control of the optical unit temperature in the range of 5 C above ambient to 55 CC minimizes changes in refractive index due to temperature variations The eluent flows through the sample cell and via the same heat exchanger to the purge valve With the purge valve in the OFF position the eluent passes to the recycle valve If the recycle valve is also in the OFF WASTE position the eluent will flow via the waste port into the waste container If the recycle valve is in the ON BOTTLE position the eluent will flow via the recycle port back to the solvent bottle The recycle valve can be manually set to the ON or OFF position or the Automatic recycling after analysis mode can be enabled In this mode the recycle valve will automatically switch to the ON position after each analysis has been completed and return to the OFF position before the next 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 into the recycle valve see Figure 5 on page 17 Periodically switching the purge valve to the on position while only mobile phase is
93. participating modules are switched on or properly powered one line is defined to summarize the POWER ON state of all connected modules Control of analysis is maintained by signal readiness READY for next analysis followed by START of run and optional STOP of run triggered on the respective lines In addition PREPARE and START REQUEST may be issued The signal levels are defined as e standard TTL levels 0 V is logic true 5 0 V is false fan out is 10 e input load is 2 2 kOhm against 5 0 V and output are open collector type inputs outputs wired or technique All common TTL circuits operate with a 5 V power supply A TTL signal is defined as low or L when between 0 V and 0 8 V and high or H when between 2 0 V and 5 0 V with respect to the ground terminal Agilent 1260 Infinity RID User Manual 29 1 Introduction to the Refractive Index Detector Table 3 Remote Signal Distribution Pin Signal Description 1 DGND Digital ground 2 PREPARE L Request to prepare for analysis for example calibration detector lamp on Receiver is any module performing pre analysis activities 3 START L Request to start run timetable Receiver is any module performing run time controlled activities 4 SHUT DOWN L System has serious problem for example leak stops pump Receiver is any module capable to reduce safety risk 5 Not used 6 POWER ON H All modules connected to system are switched on Receiver is any modul
94. perable as a module It only uses basic functions of the operating system for example for communication In this mode the main firmware can be loaded using update utilities Table 10 Boot Resident Settings without on board LAN Mode Select SW1 sw2 SW3 SW4 SW5 SW6 SW7 Swe LAN No LAN TEST BOOT 1 1 1 0 0 0 0 0 TEST BOOT 1 1 0 0 1 0 0 0 CAUTION Forced Cold Start A forced cold start can be used to bring the module into a defined mode with default parameter settings Loss of data Forced cold start erases all methods and data stored in the non volatile memory Exceptions are diagnosis and repair log books which will not be erased gt Save your methods and data before executing a forced cold start 36 If you use the following switch settings and power the instrument up again a forced cold start has been completed Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 Table 11 Forced Cold Start Settings without on board LAN Mode Select SW1 sw2 SW3 sSWw4 SW5 SW6 SW7 SW8 LAN TEST BOOT 1 1 0 0 0 0 0 1 No LAN TEST BOOT 1 1 0 0 1 0 0 1 Agilent 1260 Infinity RID User Manual 37 1 38 Introduction to the Refractive Index Detector Setting the 8 bit Configuration Switch On Board LAN Agilent 1260 Infinity RID User Manual s Agilent 1260 Infinity RID User Manual ee 2 Site Requirements and Specifications g 7 Site Requirements 40
95. plug to be connected to Agilent modules interface board The other end is for general purpose Agilent Module Interface Board to general purposes 11 External contact cable Color Pin Agilent Signal Name Agilent module interface module board to general purposes p n G1103 61611 White 1 EXT 1 Brown 2 EXT 1 Green 3 EXT 2 Yellow 4 EXT 2 Grey 5 EXT 3 Pink 6 EXT 3 Blue 7 EXT 4 Red 8 EXT 4 Black 9 Not connected Violet 10 Not connected Grey pink 11 Not connected Red blue 12 Not connected White green 13 Not connected Brown green 14 Not connected White yellow 15 Not connected Agilent 1260 Infinity RID User Manual 157 11 Identifying Cables External Contact Cable 158 Agilent 1260 Infinity RID User Manual Agilent 1260 Infinity RID User Manual 12 Appendix General Safety Information 160 The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC 163 Lithium Batteries Information 164 Radio Interference 165 Sound Emission 166 Solvent Information 167 Agilent Technologies on Internet 169 This chapter provides safetey and other general information ee Agilent Technologies 159 12 Appendix General Safety Information Safety Symbols Table 19 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect risk of harm to the operator and to protect the apparatus against damage In
96. pment Agilent 1260 Infinity RID User Manual 41 2 Site Requirements and Specifications Bench Space The module dimensions and weight see Table 12 on page 43 allow you to place the module on almost any desk or laboratory bench It needs an additional 2 5 cm 1 0 inches of space on either side and approximately 8 cm 3 1 inches in the rear for air circulation and electric connections If the bench should carry an Agilent system make sure that the bench is designed to bear the weight of all modules The module should be operated in a horizontal position Environment CAUTION Your detector will work within the specifications at ambient temperatures and relative humidity described in Table 12 on page 43 ASTM drift tests require a temperature change below 2 C hour 3 6 F hour over one hour period Our published drift specification refer also to Performance Specifications on page 44 is based 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 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 The module is designed to operate in a typical electromagnetic environment EN61326 1 where RF transmitters such as mobile phones should not be used in close proximity
97. s 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 relation to the changes in medium density The density of a medium will be affected by the following factors Composition if not a pure substance Temperature Pressure Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 Detection Principle Detector Design The Agilent 1260 Infinity Refractive Index Detector is a differential refractometer that measures the deflection of a light beam due to the difference in refractive index between 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 which produces an electrical current proportional to the amount of light that falls upon it see Figure 3 on page 14 Agilent 1260 Infinity RID User Manual 13 1 14 Introduction to the Refractive Index Detector Diode 1 Diode 2 Zero glass Light receiver Reference cell Mirr
98. sconnected Please contact your Agilent service representative 2 Defective recycle valve Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative Agilent 1260 Infinity RID User Manual 111 7 Error Information Lamp Voltage too Low Probable cause 1 Defective main board 2 Defective lamp or optics Lamp Voltage too High Probable cause 1 Contaminated flow cell 2 Defective main board 3 Defective lamp or optics Lamp Current too High Probable cause 1 Defective main board 2 Defective lamp or optics 112 Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Suggested actions Flush the flow cell Please contact your Agilent service representative Please contact your Agilent service representative Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Agilent 1260 Infinity RID User Manual Error Information 7 Lamp Current too Low Probable cause Suggested actions 1 Optical unit cable disconnected Please contact your Agilent service representative 2 Defective main board Please contact your Agilent service representative 3 Defective lamp or optics Please contact your Agilent service representative Wait Function Timed Out Wait for temperature or wait for defined
99. signal has not been fulfilled within the specified time frame Probable cause Suggested actions 1 Time too short Increase time Agilent 1260 Infinity RID User Manual 113 7 Error Information Not Ready Messages Not ready messages are displayed during the wait for a specific condition to be reached or completed or while a self test procedure is running In the event of such a failure the yellow status indicator at the front of the detector is switched ON This section describes the meaning of detector not ready messages Purge Time Running Probable cause Suggested actions 1 The purge valve is open liquid is flowing Allow the reference purge time to elapse through both sample and reference cell Wait for Purge Probable cause Suggested actions 1 The detector is waiting after the automatic Allow the wait time to elapse purge of the reference cell 114 Agilent 1260 Infinity RID User Manual Error Information 7 Unbalanced Diodes Probable cause Suggested actions 1 The diode balance value is outside the e Flush the reference cell with the mobile pre set range 0 5 to 0 5 an unequal phase being used amount of light is falling on the two light Perform the RID Optical Balance procedure receiving diodes see The Optical Balance Procedure on page 124 Not Enough Light Probable cause Suggested actions 1 There is insufficient light falling on the light Flush the flow cell with the mobile phase being receiv
100. t chromatogram 126 timeout 100 troubleshooting errormessages 90 90 99 status indicators 90 92 U unpacking 48 user interfaces 94 using EMF 21 using the detector optimization 64 using the detector detector control 66 detector settings 68 more settings 70 optimization 84 Agilent 1260 Infinity RID User Manual 173 www agilent com In This Book This manual contains technical reference information about the Agilent 1260 Infinity Refractive Index Detector G1362 introduction e specifications e installation configuration e optimizing e troubleshooting and diagnostics maintenance e parts identification e safety and related information Agilent Technologies 2010 2012 Printed in Germany 05 12 G1362 90011 Rev B fe Agilent Technologies
101. t supplied by the vendor and follow good laboratory practice gt The amount of substances should be reduced to the minimal volume required for the analysis gt Do not operate the instrument in an explosive atmosphere The flow cell is shipped with a filling of isopropanol also recommended when the instrument and or flow cell is shipped to another location This is to avoid breakage due to subambient conditions Agilent 1260 Infinity RID User Manual 59 3 Installing the Refractive Index Detector Flow Connections 1 Press the release buttons and remove the front cover to 2 Locate the in waste and recycle ports gain access to the interface port area 3 Remove the blanking plug and connect the interfacing 4 Remove the blanking plug and connect one of the tubes capillary to the N port from the interface tubing kit to the waste port 60 Agilent 1260 Infinity RID User Manual Installing the Refractive Index Detector 3 The back pressure rating of the refractive index flow cell is 5 bar Therefore the RI detector must be the last module in the flow path If an additional detector is to be installed it must be connected upstream of the refractive index detector in order to avoid damage to the RID flow cell due to overpressure 5 Remove the blanking plug and connect the other tube from the interface tubing kit to the recycle port ST U eT
102. ternary pump bypass the MCGV in the quaternary pump You have to virtually convert the quaternary pump into an isocratic one by directly connecting the solvent inlet tubing from degasser or solvent bottle to the active inlet valve of the pump use PEEK adapter 1 4 28 to 10 32 p n 0100 1847 which is delivered with the accessory kit of the detector 12 Consider solvent changes with time Baseline drift can be caused by the tendency of certain solvents to change over time For example the acetonitrile content of acetonitrile water mixtures will decrease tetrahydrofuran will form peroxides the amount of water in hygroscopic organic solvents will increase and solvents such as tetrahydrofuran held in the reference cell may begin to regas Agilent 1260 Infinity RID User Manual 85 5 86 Optimizing the Refractive Index Detector 13 Eliminate mobile phase column combination problems Certain mobile phases in combination with specific columns can generate long term baseline noise For example acetonitrile water mobile phases with certain aminopropyl bonded phase columns To eliminate the combination of mobile phase and column as a cause of long term noise replace the column with Restriction capillary p n G1362 87301 and re evaluate the detector performance Potential Causes for Baseline Problems Noise short term Typically the sources for short term noise are either electronic check the settings for the peak widths check for ambie
103. with a 9 pin male SUB D type connector The pins are defined as Agilent 1260 Infinity RID User Manual 27 1 28 Introduction to the Refractive Index Detector Table 2 RS 232C Connection Table Pin Direction Function 1 In DCD 2 In RxD 3 Out TxD 4 Out DTR 5 Ground 6 In DSR 7 Out RTS 8 In CTS 9 In RI Instrument PC DCD 1 1 DCD RX 2 2 RX TX 3 xX 3 x DTR 4 s 4 DTR GND 5 X 5 GND DSR 6 6 DSR RTS 7 X 7 RTS CTS 8 8 CTS RI 9 9 RI DB9 DB9 DB9 DB9 Male Female Female Male Figure 10 RS 232 Cable Analog Signal Output The analog signal output can be distributed to a recording device For details refer to the description of the module s main board Agilent 1260 Infinity RID User Manual Introduction to the Refractive Index Detector 1 APG Remote The APG Remote connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features as common shut down prepare and so on Remote control allows easy connection between single instruments or systems to ensure coordinated analysis with simple coupling requirements The subminiature D connector is used The module provides one remote connector which is inputs outputs wired or technique To provide maximum safety within a distributed analysis system one line is dedicated to SHUT DOWN the system s critical parts in case any module detects a serious problem To detect whether all
104. x range Measurement range Optical zeroing Optics temperature control Sample cell Valves Volumes Liquid contact materials pH range Performance specifications Time programmable parameters Detector zero Refractive Index 1 00 1 75 RIU calibrated 600 x 10 RIU via set screw 5 C above ambient to 55 C volume 8 pL maximum pressure 5 bar 0 5 Mpa maximum flow rate 5 mL min Automatic purge and automatic solvent recycle Inlet port to sample cell 62 pL inlet port to outlet port 590 pL 316 stainless steel PTFE and quartz glass 2 3 9 5 Short term noise see note below this table lt 2 5x 10 RIU Drift lt 200 x 10 RIU h polarity peak width automatic zero before analysis Agilent 1260 Infinity RID User Manual Site Requirements and Specifications 2 Table 13 Performance Specifications Agilent 1260 Infinity Refractive Index Detector Type Specification Comments Control and data evaluation Analog outputs Communications Safety and maintenance GLP features Housing Parameter entry signal display on line help and diagnostics with the Agilent 1260 Infinity Control Module Optional PCMCIA card for method sequence and logbook storage and transfer Agilent ChemStation for LC PC based software for control and data evaluation Recorder integrator 100 mV or 1 V output range selectable one output Controller area network CAN LAN R
105. ze leeg zijn moet u ze niet weggooien maar inleveren als KCA Agilent 1260 Infinity RID User Manual Appendix 12 Radio Interference Cables supplied by Agilent Technologies are screened to provide optimized protection against radio interference All cables are in compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with unscreened cables or used for measurements on open set ups the user has to assure that under operating conditions the radio interference limits are still met within the premises Agilent 1260 Infinity RID User Manual 165 12 Appendix Sound Emission Manufacturer s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991 This product has a sound pressure emission at the operator position lt 70 dB e Sound Pressure Lp lt 70 dB A e At Operator Position e Normal Operation e According to ISO 7779 1988 EN 27779 1991 Type Test 166 Agilent 1260 Infinity RID User Manual Appendix 12 Solvent Information Flow Cell To protect optimal functionality of your flow cell e Avoid the use of alkaline solutions pH gt 9 5 which can attack quartz and thus impair the optical properties of the flow cell e Ifthe flow cell is transported while temperatures are below 5 C it must be assured that the cell is filled with alcohol e Aqueous solvents in the flow cell can bu

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