Agilent 1260 Infinity Refractive Index Detector - User Manual
Agilent Technologies
G1362-90011 RID-A USR EN User Manual
Agilent 1260 Infinity Refractive Index Detector
Agilent Technologies
Notices
© Agilent Technologies, Inc. 2010, 2012
No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws.
Manual Part Number
G1362-90011 Rev. B
Edition
05/12
Printed in Germany
Agilent Technologies Hewlett-Packard-Strasse 8 76337 Waldbronn
This product may be used as a component of an in vitro diagnostic system if the system is registered with the appropriate authorities and complies with the relevant regulations. Otherwise, it is intended only for general laboratory use.
Warranty
The material contained in this document is provided "as is," and is subject to being changed, without notice, in future editions. Further, to the maximum 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 particular purpose. Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing, use, or performance of this document or of any information contained herein. Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate agreement shall control.
Technology Licenses
The hardware and/or software described in this document are furnished under a license and may be used or copied only in accordance 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 subcontract, Software is delivered and licensed as "Commercial computer software" as defined in DFAR 252.227-7014 (June 1995), or as a "commercial item" as defined in FAR 2.101(a) or as "Restricted computer software" as defined in FAR 52.227-19 (June 1987) or any equivalent agency regulation or contract clause. Use, duplication or disclosure 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 performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met.
WARNING
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 indicated conditions are fully understood 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 different 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
3
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
1 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
2 Site Requirements and Specifications 39 Site Requirements 40 Physical Specifications 43 Performance Specifications 44
3 Installing the Refractive Index Detector 47 Unpacking the Detector 48 Optimizing the Stack Configuration 51 Installing the Detector 56 Flow Connections 59
4 Using the Refractive Index Detector 63 Operation of the Refractive Index Detector 64 Running a Checkout Sample 72 Checking Baseline Noise and Drift 76
5 Optimizing the Refractive Index Detector 83 Refractive Index Detector Optimization 84
Agilent 1260 Infinity RID User Manual
5
Contents
6 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
7 Error Information 97 What Are Error Messages 99 General Error Messages 100 Refractive Index Detector Specific Error Messages 107 Not-Ready Messages 114
8 Test Functions 117 Refractive Index Calibration 118 Optical Balance 123 Using the Build-in Test Chromatogram 126
9 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
6
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 Emission 166 Solvent Information 167 Agilent Technologies on Internet 169
Agilent 1260 Infinity RID User Manual
7
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.
Agilent Technologies
9
1 Introduction to the Refractive Index Detector
Introduction to the Refractive Index Detector
Introduction to the Refractive Index Detector
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 troubleshooting · 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
10
Agilent 1260 Infinity RID User Manual
How the Detector Operates
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.
Where: · n = Refractive index of medium 1 relative to medium 2 · n2 = Refractive index of medium 2 · n1 = Refractive index of medium 1 · 1 = angle of incident light in medium 1 · 2 = angle of refraction in medium 2
Medium 1
Figure 2 Light Refraction Agilent 1260 Infinity RID User Manual
Medium 2 11
1 Introduction to the Refractive Index Detector
How the Detector Operates
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.
Where: · = angle of external deflection · n2 = Refractive index of medium 2 · n1 = Refractive index of medium 1
Factors that Affect Refractive Index
The refractive index of a medium is affected by a number of factors; 1 Wavelength
The refractive index varies with changes in the wavelength of the incident light beam. 2 Density As the density of the medium changes the refractive index changes. At a fixed wavelength of incident light the changes in refractive index are generally linear in 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
12
Agilent 1260 Infinity RID User Manual
Detection Principle
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 Introduction to the Refractive Index Detector
Detection Principle
9^dYZ&
9^dYZ'
A^\]igZXZ^kZg
OZgd\aVhh
GZ[ZgZcXZXZaa
HVbeaZXZaa
B^ggdg
Figure 3
Ha^i 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.
14
Agilent 1260 Infinity RID User Manual
Introduction to the Refractive Index Detector 1
Detection Principle
AVbe 8dcYZchZgaZch >cX^YZcia^\]i 9^dYZh OZgd\aVhh 9Z[aZXiZYa^\]i 8daa^bVidgaZch HVbeaZXZaa GZ[ZgZcXZXZaa B^ggdg
Figure 4 Optical Path
Agilent 1260 Infinity RID User Manual
15
1 Introduction to the Refractive Index Detector
Flow Path
Flow Path
The column eluent enters the optical unit through the in port 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 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.
16
Agilent 1260 Infinity RID User Manual
Introduction to the Refractive Index Detector 1
Flow Path
5
(
+ -
(
)
. Figure 5
,
&
Flow Path
'
;adleVi]l^i]ejg\ZkVakZdc ;adleVi]l^i]ejg\ZkVakZd[[
1
Flow in
2
Heater
3
Heat exchanger
4
Sample cell
5
Purge valve
6
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
Flow Path
from optical unit sample cell (top right)
(1)
to optical unit sample cell (bottom right)
(2)
8DB28DBBDC CD2CDGB6AANDE:C C82CDGB6AAN8ADH:9
8DCC:8I>C<EDGIH
>C
Metal union block
L6HI:
(3)
(4)
G:8N8A:
Purge valve
CD
C8
8DB
8DB
C8
CD
Recycle valve
top left bottom left optical unit (from and to reference cell)
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
BZiVajc^dc
*
WadX`
Introduction to the Refractive Index Detector 1
Flow Path
Ejg\ZkVakZ 8DB
GZXnXaZkVakZ 8DB
C8
CD
C8
CD
HVbeaZXZaa
8DB28DBBDC CD2CDGB6AANDE:C C82CDGB6AAN8ADH:9 >C
GZ[ZgZcXZ XZaa
G:8N8A: L6HI:
Figure 7 Flow path with the Purge- and Recycle-Valves = OFF
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
BZiVajc^dc WadX`
Ejg\ZkVakZ 8DB
GZXnXaZkVakZ 8DB
C8
CD
C8
CD
HVbeaZXZaa
8DB28DBBDC
CD2CDGB6AANDE:C
>C
8DB2CDGB6AAN8ADH:9
GZ[ZgZcXZ XZaa
G:8N8A: L6HI:
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
Early Maintenance Feedback
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 maintenance 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
Instrument Layout
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: · virtual elimination of fixing screws, bolts or ties, reducing the number of
components and increasing the speed of assembly/disassembly, · the plastic layers have air channels molded into them so that cooling air can
be guided exactly to the required locations, · the plastic layers help cushion the electronic and mechanical parts from
physical shock, and · the metal inner cabinet shields the internal electronics from
electromagnetic interference and also helps to reduce or eliminate radio frequency emissions from the instrument itself.
22
Agilent 1260 Infinity RID User Manual
Electrical Connections
Introduction to the Refractive Index Detector 1
Electrical Connections
NOTE
· 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.
· 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.
· 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.
· The power input socket accepts a line voltage of 100 240 VAC ± 10 % with a 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 Technologies 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
NOTE
Figure 9 Rear View of Detector Electrical Connections and Label The GPIB interface has been removed with the introduction of the 1260 Infinity modules.
Serial Number Information
The serial number information on the instrument labels provide the following information:
CCXZZ00000 CC X ZZ
00000
Format
Country of manufacturing (DE Germany)
Alphabetic character A-Z (used by manufacturing)
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)
Serial number
24
Agilent 1260 Infinity RID User Manual
Interfaces
Introduction to the Refractive Index Detector 1
Interfaces
The Agilent 1200 Infinity Series modules provide the following interfaces:
Table 1 Agilent 1200 Infinity Series Interfaces
Module
CAN
Pumps
G1310B Iso Pump
2
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
G1361A Prep Pump
2
Samplers
G1329B ALS
2
G2260A Prep ALS
G1364B FC-PS
2
G1364C FC-AS
G1364D FC-S
G1367E HiP ALS
G1377A HiP micro ALS
G2258A DL ALS
G4226A ALS
2
Detectors
G1314B VWD VL
2
G1314C VWD VL+
G1314E/F VWD
2
LAN/BCD LAN
RS-232 Analog APG
(optional) (on-board)
Remote
Yes
No
Yes
1
Yes
No
Yes
Yes
No
Yes
Yes
No
Yes
No
Yes
Yes
No
Yes
No
Yes
Yes
No
Yes
No
Yes
Yes
No
Yes
No
Yes
Yes
No
Yes
1
Yes
No
Yes
Yes
1
Yes
Special
CAN-DC- OUT for CAN slaves THERMOSTAT for G1330B THERMOSTAT for G1330B CAN-DC- OUT for CAN slaves
Agilent 1260 Infinity RID User Manual
25
1 Introduction to the Refractive Index Detector
Interfaces
Table 1 Agilent 1200 Infinity Series Interfaces
Module
G4212A/B DAD G1315C DAD VL+ G1365C MWD G1315D DAD VL G1365D MWD VL G1321B FLD G1362A RID G4280A ELSD
Others G1316A/C TCC G1322A DEG G1379B DEG G4227A Flex Cube G4240A CHIP CUBE
CAN LAN/BCD LAN
RS-232 Analog APG
Special
(optional) (on-board)
Remote
2
No
Yes
Yes
1
Yes
2
No
Yes
Yes
2
Yes
2
Yes
No
Yes
1
Yes
No No
No
Yes
Yes
Yes
EXT Contact
AUTOZERO
2
No
No
Yes
No
Yes
No No
No
No
No
Yes
AUX
No No
No
Yes
No
No
AUX
2
No
No
No
No
No
2
Yes
No
Yes
No
Yes
CAN-DC- OUT for CAN
slaves
THERMOSTAT for
G1330A/B (NOT USED)
NOTE
The detector (DAD/MWD/FLD/VWD/RID) is the preferred access point for control via LAN. The inter-module communication is done via CAN.
· CAN connectors as interface to other modules · LAN connector as interface to the control software · RS-232C as interface to a computer · REMOTE connector as interface to other Agilent products · Analog output connector(s) for signal output
26
Agilent 1260 Infinity RID User Manual
Introduction to the Refractive Index Detector 1
Interfaces
Overview Interfaces
NOTE
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.
NOTE
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 · 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) with a 9-pin male SUB-D type connector. The pins are defined as:
Agilent 1260 Infinity RID User Manual
27
1 Introduction to the Refractive Index Detector
Interfaces
Table 2 RS-232C Connection Table
Pin
Direction
1
In
2
In
3
Out
4
Out
5
6
In
7
Out
8
In
9
In
Function DCD RxD TxD DTR Ground DSR RTS CTS RI
>chigjbZci
E8
BVaZ ;ZbVaZ
;ZbVaZ BVaZ
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.
28
Agilent 1260 Infinity RID User Manual
NOTE
Introduction to the Refractive Index Detector 1
Interfaces
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 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: · standard TTL levels (0 V is logic true, + 5.0 V is false), · fan-out is 10, · 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
Interfaces
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 module 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)
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: · Default is ALL switches DOWN (best settings) - Bootp mode for LAN. · 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.
NOTE
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 Configuration.
Agilent 1260 Infinity RID User Manual
31
1 Introduction to the Refractive Index Detector
Setting the 8-bit Configuration Switch (On-Board LAN)
Table 4 8-bit Configuration Switch (with on-board LAN)
Mode
SW 1
SW 2
LAN
0
0
Auto-negotiation
10 MBit, half-duplex
10 MBit, full-duplex
100 MBit, half-duplex
100 MBit, full-duplex
Bootp
Bootp & Store
Using Stored
Using Default
TEST
1
1
Boot Resident System
Revert to Default Data (Coldstart)
Function
SW 3
SW 4 SW 5
Link Configuration
0
x
x
1
0
0
1
0
1
1
1
0
1
1
1
x
x
x
x
x
x
x
x
x
x
x
x
System
1
x
x
x
SW 6
SW 7
SW 8
Init Mode Selection
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
0
0
0
0
0
1
0
1
0
0
1
1
NVRAM
x
1
NOTE
Legend:
0 (switch down), 1 (switch up), x (any position) When selecting the mode TEST, the LAN settings are: Auto-Negotiation & Using Stored.
NOTE
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 (On-Board LAN)
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.
NOTE
Figure 12 Configuration switch (settings depend on configured mode)
All modules without on-board LAN: · default is ALL DIPS DOWN (best settings) - Bootp mode for LAN · 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.
NOTE
The following tables represent the configuration switch settings for the modules without on-board LAN only.
Agilent 1260 Infinity RID User Manual
33
1 Introduction to the Refractive Index Detector
Setting the 8-bit Configuration Switch (On-Board LAN)
Table 5 8-bit Configuration Switch (without on-board LAN)
Mode Select
1
RS-232C
0
Reserved
1
TEST/BOOT
1
2
3
4
5
6
7
8
1
Baudrate
Data
Parity
Bits
0
Reserved
1
RSVD
SYS
RSVD RSVD FC
NOTE
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.
Table 6 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 selecting 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.
34
Agilent 1260 Infinity RID User Manual
Introduction to the Refractive Index Detector 1
Setting the 8-bit Configuration Switch (On-Board LAN)
Table 7 Baudrate Settings (without on-board LAN)
Switches
3
4
5
0
0
0
0
0
1
0
1
0
0
1
1
Baud Rate
9600 1200 2400 4800
Switches
3
4
5
1
0
0
1
0
1
1
1
0
1
1
1
Baud Rate
9600 14400 19200 38400
Table 8 Data Bit Settings (without on-board LAN)
Switch 6 0 1
Data Word Size 7 Bit Communication 8 Bit Communication
Table 9 Parity Settings (without on-board LAN)
Switches
7
8
0
0
1
0
1
1
Parity
No Parity Odd Parity 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
Setting the 8-bit Configuration Switch (On-Board LAN)
Special Settings
The special settings are required for specific actions (normally in a service case).
NOTE
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 operable 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)
LAN No LAN
Mode Select SW1 SW2 SW3 SW4 SW5 SW6 SW7 SW8
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.
Save your methods and data before executing a forced cold start.
If you use the following switch settings and power the instrument up again, a forced cold start has been completed.
36
Agilent 1260 Infinity RID User Manual
Introduction to the Refractive Index Detector 1
Setting the 8-bit Configuration Switch (On-Board LAN)
Table 11 Forced Cold Start Settings (without on-board LAN)
LAN No LAN
Mode Select SW1 SW2 SW3 SW4 SW5 SW6 SW7 SW8
TEST/BOOT 1
1
0
0
0
0
0
1
TEST/BOOT 1
1
0
0
1
0
0
1
Agilent 1260 Infinity RID User Manual
37
1 Introduction to the Refractive Index Detector
Setting the 8-bit Configuration Switch (On-Board LAN)
38
Agilent 1260 Infinity RID User Manual
Agilent 1260 Infinity RID User Manual
2 Site Requirements and Specifications
Site Requirements 40 Physical Specifications 43 Performance Specifications 44
This chapter provides information on environmental requirements, physical and performance specifications.
Agilent Technologies
39
2 Site Requirements and Specifications
Site Requirements
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.
WARNING
Hazard of electrical shock or damage of your instrumentation can result, if the devices are connected to a line voltage higher than specified. Connect your instrument to the specified line voltage only.
WARNING
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.
Always unplug the power cable before opening the cover.
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.
Make sure the power connector of the instrument can be easily reached and unplugged.
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
Site Requirements
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.
WARNING
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.
Never operate your instrumentation from a power outlet that has no ground connection.
Never use a power cord other than the Agilent Technologies power cord designed for your region.
WARNING
Use of unsupplied cables
Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury.
Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
WARNING
Unintended use of supplied power cords
Using power cords for unintended purposes can lead to personal injury or damage of electronic equipment.
Never use the power cords that Agilent Technologies supplies with this instrument for any other equipment.
Agilent 1260 Infinity RID User Manual
41
2 Site Requirements and Specifications
Site Requirements
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
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.
NOTE
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.
CAUTION
Condensation within the module Condensation will damage the system electronics.
Do not store, ship or use your module under conditions where temperature fluctuations could cause condensation within the module.
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
Physical Specifications
Site Requirements and Specifications 2
Physical Specifications
Table 12 Physical Specifications
Type Weight Dimensions (height × width × depth) Line voltage Line frequency Power consumption Ambient operating temperature Ambient non-operating temperature Humidity Operating Altitude Non-operating altitude Safety standards: IEC, CSA, UL
Specification
Comments
17 kg (38 lbs)
180 x 345 × 435 mm (7 x 13.5 × 17 inches)
100 240 VAC, ± 10% 50 or 60 Hz, ± 5% 160 VA / 65 W / 222 BTU 055 °C (32131 °F)
Wide-ranging capability Maximum
-4070 °C (-4158 °F)
< 95%, at 2540 °C (77104 °F)
Non-condensing
Up to 2000 m (6562 ft)
Up to 4600 m (15091 ft)
For storing the module
Installation Category II, Pollution Degree 2 For indoor use only.
Agilent 1260 Infinity RID User Manual
43
2 Site Requirements and Specifications
Performance Specifications
Performance Specifications
Table 13 Performance Specifications Agilent 1260 Infinity Refractive Index Detector
Type
Specification
Comments
Detection type
Refractive Index
Refractive index range 1.00 - 1.75 RIU, calibrated
Measurement range +/- 600 x 10-6 RIU
Optical zeroing
via set screw
Optics temperature control
5 °C above ambient to 55 °C
Sample cell
volume 8 µL maximum pressure 5 bar (0.5 Mpa) maximum flow rate 5 mL/min
Valves
Automatic purge and automatic solvent recycle
Volumes
Inlet port to sample cell 62 µL, inlet port to outlet port 590 µL
Liquid contact materials 316 stainless steel, PTFE and quartz glass
pH range
2.3 - 9.5
Performance specifications
Short term noise < +/- 2.5 x 10-9 RIU Drift < 200 x 10-9 RIU/h
see note below this table
Time programmable parameters
polarity, peak width
Detector zero
automatic zero before analysis
44
Agilent 1260 Infinity RID User Manual
Site Requirements and Specifications 2
Performance Specifications
Table 13 Performance Specifications Agilent 1260 Infinity Refractive Index Detector
Type
Specification
Comments
Control and data evaluation
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.
Analog outputs
Recorder/integrator: 100 mV or 1 V, output range selectable, one output
Communications
Controller-area network (CAN), LAN, RS-232C, APG Remote: ready, start, stop and shut-down signals
Safety and maintenance
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.
GLP features
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 (OQ/PV).
Housing
All materials recyclable.
Agilent 1260 Infinity RID User Manual
45
2 Site Requirements and Specifications
Performance Specifications
Table 13 Performance Specifications Agilent 1260 Infinity Refractive Index Detector
Type Environment
Dimensions
Weight
Specification
Comments
0 to 55 °C constant temperature at < 95% humidity (non-condensing)
180 mm x 345 mm x 435 mm (7 x 13.5 x 17 inches) (height x width x depth)
17 kg (38 lbs)
NOTE
Based on ASTM method E-1303-95 Practice for Refractive Index Detectors used in Liquid Chromatography. Reference conditions; optics temperature 35 °C, response time 4 s, flow 1.0 mL/min LC-grade Water, restriction capillary, column compartment temperature 35 °C, Agilent on-line degasser G1322A, pump and thermostatted column compartment. Instrument equilibrated for 2 hours.
46
Agilent 1260 Infinity RID User Manual
Agilent 1260 Infinity RID User Manual
3 Installing the Refractive 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.
Agilent Technologies
47
3 Installing the Refractive Index Detector
Unpacking the 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.
Notify your Agilent sales and service office about the damage.
An Agilent service representative will inspect the instrument at your site and initiate appropriate actions.
Delivery Checklist
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 service office.
Table 14 Delivery Checklist 1260 RID
Description Detector Power cable User Manual (on User Documentation CD) Accessory kit (p/n G1362-68755)
Quantity 1 1 1 1
48
Agilent 1260 Infinity RID User Manual
Installing the Refractive Index Detector 3
Unpacking the Detector
Accessory Kit
Accessory kit (p/n G1362-68755) contains some accessories needed for the installation of the detector.
p/n G1362-68706 G1362-87300 G1362-87301 5181-1516 0100-1847
Description Interface tubing kit Interfacing capillary Restriction capillary CAN cable, Agilent module to module, 0.5 m PEEK adapter 1/4-28 to 10-32 (Adapter AIV to solvent inlet tubes)
(
'
&
Figure 13 Interface Tubing Kit Parts )
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
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 Configuration
HdakZciXVW^cZi KVXjjbYZ\VhhZg Ejbe
6jidhVbeaZg
>chiVcie^adi
8dajbcXdbeVgibZci
9ZiZXidg
Figure 16 Recommended Stack Configuration (Front View)
52
Agilent 1260 Infinity RID User Manual
Installing the Refractive Index Detector 3
Optimizing the Stack Configuration
GZbdiZXVWaZ 6cVad\h^\cVaejbeegZhhjgZ 86C7jhXVWaZ
86C7jhXVWaZ
68edlZg
6cVad\h^\cVaYZiZXidg
A6CidXdcigdahd[ilVgZ gZfj^gZh >ciZg[VXZXVgY<&(+.7
68edlZg
Figure 17 Recommended Stack Configuration (Rear View)
Agilent 1260 Infinity RID User Manual
53
3 Installing the Refractive Index Detector
Optimizing the Stack Configuration
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).
>chiVciE^adi
9ZiZXidg
8dajbcXdbeVgibZci
6jidhVbeaZg
I]ZgbdhiVi[dgi]Z6AH dei^dcVa
HdakZciXVW^cZi 9Z\VhhZgdei^dcVa Ejbe
Figure 18 Recommended Two Stack Configuration for 1260 (Front View)
54
Agilent 1260 Infinity RID User Manual
A6CidXdcigdahd[ilVgZ 86C7jhXVWaZ id>chiVciE^adi
I]ZgbdXVWaZ dei^dcVa
Installing the Refractive Index Detector 3
Optimizing the Stack Configuration
GZbdiZXVWaZ
68EdlZg
86C7jhXVWaZ 68EdlZg
68EdlZg
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
Installing the Detector
Parts required
Description Power cord
For other cables see "Cable Overview" on page 146
Hardware required Agilent 1260 Infinity Refractive Index Detector (G1362A)
Preparations
· Locate bench space · Provide power connections · Unpack the detector
NOTE
The detector is turned on when the line power switch is pressed and the green indicator lamp is illuminated. The detector is turned off when the line power switch is protruding and the green light is OFF.
WARNING
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.
Make sure that it is always possible to access the power plug.
Remove the power cable from the instrument before opening the cover.
Do not connect the power cable to the Instrument while the covers are removed.
NOTE
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.
56
Agilent 1260 Infinity RID User Manual
Installing the Refractive Index Detector 3
Installing the Detector
HiVijh^cY^XVidg \gZZc$nZaadl$gZY
3 Ensure the line power switch at the front of the detector is OFF.
A^cZedlZg hl^iX]l^i]\gZZca^\]i
Figure 20 Front View of Detector
4 Connect the power cable to the power connector at the rear of the detector. 5 Connect the CAN cable to other Agilent modules. 6 If an Agilent ChemStation is the controller, connect 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
86C GH'(' 6E<gZbdiZ
6cVad\h^\cVa
9 Turn ON power by pushing the button at the lower left hand side of the detector. The status LED should be green.
8dc[^\jgVi^dc
EdlZg HZXjg^inaZkZg
NOTE
Figure 21 Rear View of Detector
The GPIB interface has been removed with the introduction of the Agilent 1260 Infinity modules
58
Agilent 1260 Infinity RID User Manual
Flow Connections
Installing the Refractive Index Detector 3
Flow Connections
Tools required
¼ inch wrench
Parts required
# p/n 1 G1362-68706 1 G1362-87300
Description Interface tubing kit Interfacing capillary
Hardware required Other modules
Preparations
WARNING
· Detector is installed in the LC system.
Toxic, flammable and hazardous solvents, samples and reagents The handling of solvents, samples and reagents can hold health and safety risks.
When working with these substances observe appropriate safety procedures (for example by wearing goggles, safety gloves and protective clothing) as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice.
The amount of substances should be reduced to the minimal volume required for the analysis.
Do not operate the instrument in an explosive atmosphere.
NOTE
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 capillary to the IN port.
GZXnXaZ LVhiZ
>c
4 Remove the blanking plug and connect one of the tubes from the interface tubing kit to the waste port.
60
Agilent 1260 Infinity RID User Manual
Installing the Refractive Index Detector 3
Flow Connections
NOTE
The back pressure rating of the refractive index flow
5 Remove the blanking plug and connect the other tube from the interface tubing kit to the recycle port.
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.
NOTE
6 Direct the waste tube into a suitable waste container. Make sure that there is no restriction of this tube.
Remove all blanking plugs from all outlet ports (waste
& recycle) of the detector to avoid potential damage to 7 If solvent recycling is to be used direct the recycle tube
the flow cell, if the recycle valve is accidentally switched to one of these ports, while flow is applied to
into the solvent bottle. Make sure that there is no restriction of this tube.
the detector.
8 Establish flow and observe if leaks occur.
NOTE
To optimize detector performance the waste container and solvent bottle should be positioned above the level of the refractive index detector and solvent pump (e.g. in the solvent compartment). This will maintain a slight pressure in the sample cell. Route the tubing behind the front covers of the modules in the stack.
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
4 Using the Refractive Index Detector
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
Running 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.
Agilent Technologies
63
4 Using the Refractive Index Detector
Operation of the Refractive Index Detector
Operation of the Refractive Index Detector
This chapter can be used for · preparing the system, · to learn the set up of an HPLC analysis and · to use it as an instrument check to demonstrate that all modules of the
system are correctly installed and connected. It is not a test of the instrument performance. · Learn about special settings
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
Operation of the Refractive Index Detector
Table 15 Choice of Priming Solvents for Different Purposes
Activity After an installation
Solvent Isopropanol
When switching between reverse phase and normal phase (both times)
After an installation
Isopropanol Ethanol or Methanol
To clean the system when using buffers
After a solvent change
Bidistilled water Bidistilled water
After the installation of normal phase Hexane + 5 % Isopropanol seals (P/N 0905-1420)
Comments
Best solvent to flush air out of the system
Best solvent to flush air out of the system
Alternative to Isopropanol (second choice)if no Isopropanol is available
Best solvent to re-dissolve buffer crystals
Best solvent to re-dissolve buffer crystals
Good wetting properties
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 Using the Refractive Index Detector
Operation of 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.
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.
· 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.
66
Agilent 1260 Infinity RID User Manual
Using the Refractive Index Detector 4
Operation of the Refractive Index Detector
· 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 cell 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
Operation of 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.
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.
· 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.
68
Agilent 1260 Infinity RID User Manual
Using the Refractive Index Detector 4
Operation of the Refractive Index Detector
· 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 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.
· 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
Operation of 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 select Setup RID signal from the Instrument menu. The More button displays additional Menus.
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
Operation of the Refractive Index Detector
Diode 1 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 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.
· 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.
· 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 Using the Refractive Index Detector
Running a Checkout Sample
Running a Checkout Sample
When Parts required
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 1 993967-902 1 01080-68704
Description Zorbax Eclipse XDB C18, 150mm x 4.6mm i.d. 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 Column Sample Flow rate Stroke A Stop time Injection volume Column compartment temperature Optical unit Temperature Polarity Peak Width (Response time)
30% Water, 70% Acetonitrile Zorbax Eclipse XDB C18, 150 mm x 4.6 mm i.d. Isocratic standard sample 1.5 ml/min 20 µl 10 min 20 µl 25 °C 35 °C Positive 0.2 min (4 s, standard)
72
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.
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:
Figure 26 RID 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
Running a Checkout Sample
The resulting chromatogram is shown in the figure below:
NOTE
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 in a 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
Checking Baseline Noise and Drift
Setting the Test Conditions
This chapter describes checking the baseline noise and drift for the Agilent 1260 Infinity Refractive Index Detector.
When
If you want to checkout the detector
Tools required
LC system with G1362A RID
Parts required
# p/n
Description
1 G1362-87301 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 Column Flow rate Compressibility Stroke Stop time Column compartment temperature Optical unit Temperature Polarity Peak Width (Response time)
LC grade water Restriction capillary 2.7 m x 0.17 mm i.d. 1.0 ml/min 46 20 µl 20 min 40 °C 40 °C Positive 0.2 min (4 s, standard)
76
Agilent 1260 Infinity RID User Manual
NOTE
Using the Refractive Index Detector 4
Checking Baseline Noise and Drift
4 Set the RID setpoints according to Figure 28 on page 77.
The optical unit temperature must be set at least 5 °C above ambient conditions. Therefore if ambient temperature is above 30 °C higher values for Optical unit Temperature and Column compartment temperature must be set.
NOTE
Figure 28 RID Baseline Check Parameters
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 User Manual
77
4 Using the Refractive Index Detector
Checking Baseline Noise and Drift
6 Specify the report style Performance + Noise as shown in Figure 29 on page 78
Figure 29 RID Baseline Check Out Report
78
Agilent 1260 Infinity RID User Manual
Using the Refractive Index Detector 4
Checking Baseline Noise and Drift 7 Set the noise determination time range to 0 - 20 minutes as shown in
Figure 30 on page 79:
Figure 30 RID Baseline Check Out Noise Ranges 8 Save the Agilent ChemStation method.
Agilent 1260 Infinity RID User Manual
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:
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
Checking Baseline Noise and Drift
11 The Agilent ChemStation report is shown in Figure 32 on page 81:
Figure 32 Baseline Check Out Results
Agilent 1260 Infinity RID User Manual
81
4 Using the Refractive Index Detector
Checking Baseline Noise and Drift
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 based 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 for 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.
82
Agilent 1260 Infinity RID User Manual
Agilent 1260 Infinity RID User Manual
5 Optimizing the Refractive Index Detector
Refractive Index Detector Optimization 84 Potential Causes for Baseline Problems 86 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
Refractive Index Detector Optimization
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 and will improve the performance of the detector.
2 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.
3 Use the correct solvents
To minimize baseline noise and drift solvents must be LC grade and filtered prior to use.
4 Check for leaks
Leaks within the LC instrument that the refractive index detector is connected to will cause problems with baseline long term noise or drift. Confirm that the instrument is free from leaks by performing the diagnostic pressure test (for the high pressure parts of the system 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.
5 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.
6 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.
84
Agilent 1260 Infinity RID User Manual
Optimizing the Refractive Index Detector 5
Refractive Index Detector Optimization
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 quaternary 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 Optimizing the Refractive Index Detector
Refractive Index Detector Optimization
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 ambient sources of electronic noise) or they are related to the solvents, their composition and flow (in order to verify this, turn off the pump, consider degassing your solvents, use only premixed solvents).
Wander (long term noise)
Excessive wander is an 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.
86
Agilent 1260 Infinity RID User Manual
Optimizing the Refractive Index Detector 5
Refractive Index Detector Optimization
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 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
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.
Agilent Technologies
89
6 Troubleshooting and Diagnostics
Overview of the Module's Indicators and Test Functions
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 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
Overview of the Module's Indicators and Test Functions
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
Status Indicators
HiVijh^cY^XVidg
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.
A^cZedlZghl^iX] l^i]\gZZca^\]i
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
Status Indicators
Module Status Indicator
The module status indicator indicates one of six possible module conditions:
· 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.
· A green status indicator, indicates the module is performing an analysis (run mode).
· A yellow indicator indicates a not-ready condition. The module is in a 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.
· 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.
· 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
User Interfaces
· Depending on the user interface, the available tests and the screens/reports may vary (see Chapter "Test Functions and Calibrations").
· 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.
· Screenshots used within these procedures are based on the Agilent Lab Advisor Software.
94
Agilent 1260 Infinity RID User Manual
Agilent Lab Advisor Software
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 User 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 Open Cover 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 too Low 112 Lamp Voltage too High 112 Lamp Current too High 112
Agilent Technologies
97
7 Error Information
Agilent Lab Advisor Software
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
What Are Error Messages
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 consumables is necessary). In the event of such a failure, the red status indicator at the front of the module is switched on, and an entry is written into the module logbook.
Agilent 1260 Infinity RID User Manual
99
7 Error Information
General Error Messages
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, and the timeout function switched off the module as requested.
Check the logbook for the occurrence and source of a not-ready condition. Restart the analysis where required.
2 A not-ready condition was present during a sequence or multiple-injection run for a period longer than the timeout threshold.
Check the logbook for the occurrence and source of a not-ready condition. Restart the analysis where required.
100
Agilent 1260 Infinity RID User Manual
Error Information 7
General Error Messages
Shut-Down
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
Suggested actions
1 Leak detected in an external instrument with Fix the leak in the external instrument before
a remote connection to the system.
restarting the module.
2 Shut-down in an external instrument with a Check external instruments for a shut-down
remote connection to the system.
condition.
3 The degasser failed to generate sufficient vacuum for solvent degassing.
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.
Remote Timeout
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.
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).
Agilent 1260 Infinity RID User Manual
101
7 Error Information
General Error Messages
Synchronization Lost
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. If one or more of the modules is no longer recognized as being connected to the system, the error message is generated.
Probable cause 1 CAN cable disconnected.
2 Defective CAN cable. 3 Defective main board in another module.
Suggested actions
· Ensure all the CAN cables are connected correctly.
· Ensure all CAN cables are installed correctly.
Exchange the CAN cable.
Switch off the system. Restart the system, and determine which module or modules are not recognized by the system.
Leak
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 1 Loose fittings. 2 Broken capillary. 3 Leaking valve. 4 Leaking flow cell.
Suggested actions Ensure all fittings are tight. Exchange defective capillaries. Exchange valve. Exchange flow cell.
102
Agilent 1260 Infinity RID User Manual
Error Information 7
General Error Messages
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 error message is generated.
Probable cause 1 Leak sensor not connected to the main
board. 2 Defective leak sensor.
3 Leak sensor incorrectly routed, being pinched by a metal component.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Please contact your Agilent service 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 1 Defective flow sensor.
Suggested actions
Please contact your Agilent service representative.
Agilent 1260 Infinity RID User Manual
103
7 Error Information
General Error Messages
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 1 Defective main board.
Suggested actions
Please contact your Agilent service representative.
Compensation 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 1 Defective main board.
Suggested actions
Please contact your Agilent service representative.
104
Agilent 1260 Infinity RID User Manual
Error Information 7
General Error Messages
Fan Failed
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.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Open Cover
The top foam has been removed. The sensor on the main board detects when the top foam is in place. If the foam is removed, the fan is switched off, and the error message is generated.
Probable cause
Suggested actions
1 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.
3 Dirty or defective sensor.
Please contact your Agilent service representative.
Agilent 1260 Infinity RID User Manual
105
7 Error Information
General Error Messages
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
Refractive Index Detector Specific Error Messages
Thermal Fuse Open
The thermal fuse of the optical unit heater has failed.
Probable cause 1 Heater cable disconnected. 2 Defective main board. 3 Defective thermal fuse.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Heater Resistance Too High
The resistance of the heater foil is above the set limit.
Probable cause 1 Heater cable disconnected. 2 Defective main board. 3 Defective heater.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Agilent 1260 Infinity RID User Manual
107
7 Error Information
Refractive Index Detector Specific Error Messages
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.
Suggested actions
Power cycle the detector.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Wrong Temperature Profile
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.
108
Agilent 1260 Infinity RID User Manual
Error Information 7
Refractive Index Detector Specific Error Messages
Undecipherable Temperature Signal
Probable cause 1 Heater cable disconnected. 2 Defective main board. 3 Defective heater.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Maximum Temperature Exceeded
The maximum heater temperature has been exceeded.
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
109
7 Error Information
Refractive Index Detector Specific Error Messages
Purge Valve Fuse Blown
The electronic fuse on the purge valve has been activated.
Probable cause 1 Short in purge valve circuit. 2 Defective purge valve.
3 Defective main board.
Suggested actions
Power cycle the module.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Recycle Valve Fuse Blown
The electronic fuse on the recycle valve has been activated.
Probable cause 1 Short in recycle valve circuit. 2 Defective recycle valve.
3 Defective main board.
Suggested actions
Power cycle the module.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
110
Agilent 1260 Infinity RID User Manual
Error Information 7
Refractive Index Detector Specific Error Messages
Purge Valve Not Connected
When activated no response was received from the purge valve.
Probable cause 1 Purge valve disconnected. 2 Defective purge valve. 3 Defective main board.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Recycle Valve Missing
When activated no response was received from the recycle valve.
Probable cause 1 Recycle valve disconnected. 2 Defective recycle valve. 3 Defective main board.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Agilent 1260 Infinity RID User Manual
111
7 Error Information
Refractive Index Detector Specific Error Messages
Lamp Voltage too Low
Probable cause 1 Defective main board.
2 Defective lamp or optics.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Lamp Voltage too High
Probable cause 1 Contaminated flow cell. 2 Defective main board.
3 Defective lamp or optics.
Suggested actions
Flush the flow cell.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Lamp Current too High
Probable cause 1 Defective main board.
2 Defective lamp or optics.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
112
Agilent 1260 Infinity RID User Manual
Lamp Current too Low
Error Information 7
Refractive Index Detector Specific Error Messages
Probable cause 1 Optical unit cable disconnected. 2 Defective main board. 3 Defective lamp or optics.
Suggested actions
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Please contact your Agilent service representative.
Wait Function Timed Out
Wait for temperature or wait for defined signal has not been fulfilled within the specified time frame.
Probable cause 1 Time too short.
Suggested actions Increase time.
Agilent 1260 Infinity RID User Manual
113
7 Error Information
Not-Ready Messages
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
1 The purge valve is open, liquid is flowing through both sample and reference cell.
Suggested actions Allow the reference purge time to elapse.
Wait for Purge
Probable cause
1 The detector is waiting after the automatic purge of the reference cell.
Suggested actions Allow the wait time to elapse.
114
Agilent 1260 Infinity RID User Manual
Unbalanced Diodes
Error Information 7
Not-Ready Messages
Probable cause
1 The diode balance value is outside the pre-set range -0.5 to + 0.5, an unequal amount of light is falling on the two light receiving diodes.
Suggested actions
· Flush the reference cell with the mobile phase being used.
· Perform the RID Optical Balance procedure (see "The Optical Balance Procedure" on page 124).
Not Enough Light
Probable cause
Suggested actions
1 There is insufficient light falling on the light receiving diodes to generate a refractive index signal.
Flush the flow cell with the mobile phase being used to ensure that it is free of air bubbles or 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
Agilent 1260 Infinity RID User Manual
8 Test Functions
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.
Agilent Technologies
117
8 Test Functions
Refractive Index Calibration
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 actual detector response, if different, to be changed to the theoretical value.
NOTE
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
Recommended after exchange of the optical unit or RIM board.
Laboratory balance
# p/n 1 1 9301-1446 1 9301-0407 1 5061-3367 1 0100-1516
Description DAB/Ph Eur/BP/JP/NF/USP Grade Sucrose Syringe Needle Sample filter Fitting male PEEK, 2/pk
118
Agilent 1260 Infinity RID User Manual
Test Functions 8
Refractive Index Calibration
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).
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
8 Test Functions
Refractive Index Calibration
c RID Calibration screen (via Calibrations).
Use the functions as described in the steps below. 4 Flushing the degasser and pump.
120
Agilent 1260 Infinity RID User Manual
Test Functions 8
Refractive Index Calibration
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. a Remove the inlet capillary or flushing syringe from the in port. b Take the syringe and fix the needle to the syringe adapter. c Suck about 1.5 mL of the calibration sample into the syringe. d Keep the syringe in a horizontal position. e Remove the needle. f Add the filter to the syringe and fit the needle to filter.
HVbeaZ[^aiZg
NOTE
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
8 Test Functions
Refractive Index Calibration
NOTE
7 Calibrate refractive index. a If the detector response differs from the theoretical response of 512,000 nRIU +/- 5,000 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.
122
Agilent 1260 Infinity RID User Manual
Optical Balance
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:
NOTE
Where: · diode1 = signal proportional to the amount of light falling on diode1 · diode2 = signal proportional to the amount of light falling on diode2
Optical balance adjustment is a manual procedure where the position of the light beam falling on the light receiving diode is adjusted using the zero glass adjustment screw.
The detector will become not-ready when the diode balance value falls outside the range 0.5 to + 0.5.
NOTE
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
123
8 Test Functions
Optical Balance
The Optical Balance Procedure
When Tools required
NOTE
When light falling on light receiving diodes is out of balance.
· 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.
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.
OZgd\aVhhVY_jhibZci hXgZlaZ[i
Figure 34 Turning the zero glass adjustment screw
Agilent 1260 Infinity RID User Manual
125
8 Test Functions
Using the Build-in Test Chromatogram
Using the Build-in Test Chromatogram
NOTE
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
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 command line: STRT
NOTE
Figure 35 Test Chromatogram with Agilent LabAdvisor 7 To stop the test chromatogram enter in the command line: STOP 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
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
This chapter provides general information on maintenance of the detector.
Agilent Technologies
129
9 Maintenance
Introduction to Maintenance
Introduction to Maintenance
NOTE
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
Warnings and Cautions
Maintenance 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.
When working with these substances observe appropriate safety procedures (for example by wearing goggles, safety gloves and protective clothing) as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice.
The amount of substances should be reduced to the minimal volume required for the analysis.
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.
Do not remove the metal top cover of the module. No serviceable parts inside. 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.
Use your Agilent products only in the manner described in the Agilent product user guides.
Agilent 1260 Infinity RID User Manual
131
9 Maintenance
Warnings and Cautions
CAUTION
Safety standards for external equipment
If you connect external equipment to the instrument, make sure that you only use accessory units tested and approved according to the safety standards appropriate for the type of external equipment.
132
Agilent 1260 Infinity RID User Manual
Detector Maintenance Procedures
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
Flow cell flushing
Leak sensor drying
Leak handling System replacement
Replacing the detector's Firmware
Typical Frequency If flow cell is contaminated. If leak has occurred. If broken or corroded.
Notes
Check for leaks. Check for leaks.
If not up to date or corrupted.
Agilent 1260 Infinity RID User Manual
133
9 Maintenance
Cleaning the Module
Cleaning the Module
WARNING
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.
Liquid dripping into the electronic compartment of your module. Liquid in the module electronics can cause shock hazard and damage the module.
Do not use an excessively damp cloth during cleaning. Drain all solvent lines before opening any fittings.
134
Agilent 1260 Infinity RID User Manual
Flow Cell Flushing
Maintenance 9
Flow Cell Flushing
When
If flow cell is contaminated
Tools required
Glass syringe, adapter
Parts required
WARNING
# 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. Wear protective gloves and goggles. Don't expose yourself to the vapors.
NOTE NOTE
NOTE
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 Tools required
If a leakage has occurred in the valve area or at the capillary connections
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
required. 5 Close the service door. 6 Replace the front cover.
KVakZhVcYijW^c\ HZgk^XZYddg
AZV`hZchdg
Figure 36 Observing for Leaks
136
Agilent 1260 Infinity RID User Manual
Maintenance 9
Replacing Leak Handling System Parts
Replacing Leak Handling System Parts
When Parts required
AZV`[jccZa ]daYZg AZV`[jccZa
If the parts are corroded or broken
# p/n 1 5061-8388 1 5041-8389 1 5042-9974
Description Leak funnel Leak funnel holder 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.
AZV`ijW^c\
AZV`hZchdg
Figure 37 Replacing Leak Handling System Parts
Agilent 1260 Infinity RID User Manual
137
9 Maintenance
Replacing the Detector's Firmware
Replacing the Detector's Firmware
When
Tools required Parts required Preparations
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 firmware might be necessary · to keep all systems on the same (validated) revision or · if a new module with newer firmware is added to a system or · if third 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.
138
Agilent 1260 Infinity RID User Manual
Replacing the Interface Board
Maintenance 9
Replacing the Interface Board
When Parts required
For all repairs inside the detector or for installation of the board
# p/n 1 G1351-68701 1 G1369B or
G1369-60002
Description Interface board (BCD) with external contacts and BCD outputs Interface board (LAN)
"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.
>ciZg[VXZWdVgY 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
10 Parts for Maintenance
Accessory Kits 142
This chapter provides information on parts for maintenance.
Agilent Technologies
141
10 Parts for Maintenance
Accessory Kits
Accessory Kits
Accessory kit (p/n G1362-68755) contains some accessories needed for the installation of the detector.
p/n G1362-68706 G1362-87300 G1362-87301 5181-1516 0100-1847
Description Interface tubing kit Interfacing capillary Restriction capillary CAN cable, Agilent module to module, 0.5 m PEEK adapter 1/4-28 to 10-32 (Adapter AIV to solvent inlet tubes)
(
'
&
Figure 39 Interface Tubing Kit Parts
)
*
Figure 40 Interfacing Capillary Parts
142
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 the Agilent 1260 Infinity LC modules.
Agilent Technologies
145
11 Identifying Cables
Cable Overview
Cable Overview
NOTE
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 35900-60750 35900-60750 01046-60105
Description Agilent module to 3394/6 integrators Agilent 35900A A/D converter Analog cable (BNC to general purpose, spade lugs)
Remote cables
p/n 03394-60600
03396-61010 5061-3378 01046-60201
Description Agilent module to 3396A Series I integrators 3396 Series II / 3395A integrator, see details in section "Remote Cables" on page 150 Agilent module to 3396 Series III / 3395B integrators Agilent module to Agilent 35900 A/D converters (or HP 1050/1046A/1049A) Agilent module to general purpose
BCD cables
p/n 03396-60560 G1351-81600
Description Agilent module to 3396 integrators Agilent module to general purpose
146
Agilent 1260 Infinity RID User Manual
Identifying Cables 11
Cable Overview
CAN cables
p/n 5181-1516 5181-1519
Description CAN cable, Agilent module to module, 0.5 m CAN cable, Agilent module to module, 1 m
LAN cables
p/n 5023-0203 5023-0202
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)
RS-232 cables
p/n G1530-60600 RS232-61600
5181-1561
Description
RS-232 cable, 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, 8 m
Agilent 1260 Infinity RID User Manual
147
11 Identifying Cables
Analog Cables
Analog Cables
One end of these cables provides a BNC connector to be connected to Agilent modules. The other end depends on the instrument to which connection is being made.
Agilent Module to 3394/6 Integrators
p/n 35900-60750
Pin 3394/6
1 2 3
Pin Agilent module
Shield Center
Signal Name
Not connected Analog Analog +
148
Agilent 1260 Infinity RID User Manual
Identifying Cables 11
Analog Cables
Agilent Module to BNC Connector
p/n 8120-1840
Pin BNC
Shield Center
Pin Agilent module
Shield
Center
Signal Name
Analog Analog +
Agilent Module to General Purpose
p/n 01046-60105
Pin 3394/6
1 2 3
Pin Agilent module
Black Red
Signal Name
Not connected Analog Analog +
Agilent 1260 Infinity RID User Manual
149
11 Identifying Cables
Remote Cables
Remote Cables
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 connected to.
Agilent Module to 3396A Integrators
p/n 03394-60600
Pin 3394
9 NC 3 NC NC NC 5,14 1 NC 13, 15
Pin Agilent module 1 - White 2 - Brown 3 - Gray 4 - Blue 5 - Pink 6 - Yellow 7 - Red 8 - Green 9 - Black
Signal Name Active (TTL)
Digital ground
Prepare run Low
Start
Low
Shut down Low
Not connected
Power on
High
Ready
High
Stop
Low
Start request Low
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.
150
Agilent 1260 Infinity RID User Manual
Identifying Cables 11
Remote Cables
Agilent Module to 3396 Series III / 3395B Integrators
p/n 03396-61010
Pin 33XX
9 NC 3 NC NC NC 14 4 NC 13, 15
Pin Agilent module 1 - White 2 - Brown 3 - Gray 4 - Blue 5 - Pink 6 - Yellow 7 - Red 8 - Green 9 - Black
Signal Name Active (TTL)
Digital ground
Prepare run Low
Start
Low
Shut down Low
Not connected
Power on
High
Ready
High
Stop
Low
Start request Low
Not connected
Agilent Module to Agilent 35900 A/D Converters
p/n 5061-3378
Pin 35900 A/D Pin Agilent module
1 - White
1 - White
2 - Brown
2 - Brown
3 - Gray
3 - Gray
4 - Blue
4 - Blue
5 - Pink
5 - Pink
6 - Yellow
6 - Yellow
7 - Red
7 - Red
8 - Green
8 - Green
9 - Black
9 - Black
Signal Name Active (TTL)
Digital ground
Prepare run Low
Start
Low
Shut down Low
Not connected
Power on
High
Ready
High
Stop
Low
Start request Low
Agilent 1260 Infinity RID User Manual
151
11 Identifying Cables
Remote Cables
Agilent Module to General Purpose
p/n 01046-60201
Pin Universal Pin Agilent module 1 - White 2 - Brown 3 - Gray 4 - Blue 5 - Pink 6 - Yellow 7 - Red 8 - Green 9 - Black
Signal Name Active (TTL)
Digital ground
Prepare run Low
Start
Low
Shut down Low
Not connected
Power on
High
Ready
High
Stop
Low
Start request Low
152
Agilent 1260 Infinity RID User Manual
BCD Cables
Identifying Cables 11
BCD Cables
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 module
Green
1
Violet
2
Blue
3
Yellow
4
Black
5
Orange
6
Red
7
Brown
8
Gray
9
Gray/pink
10
Red/blue
11
White/green 12
Brown/green 13
not connected 14
not connected 15
Signal Name BCD Digit
BCD 5
20
BCD 7
80
BCD 6
40
BCD 4
10
BCD 0
1
BCD 3
8
BCD 2
4
BCD 1
2
Digital ground Gray
BCD 11
800
BCD 10
400
BCD 9
200
BCD 8
100
+ 5 V
Low
Agilent 1260 Infinity RID User Manual
153
11 Identifying Cables
BCD Cables
Agilent Module to 3396 Integrators
p/n 03396-60560
Pin 3396
1 2 3 4 5 6 7 8 9 NC
Pin Agilent module 1 2 3 4 5 6 7 8 9 15
Signal Name BCD Digit
BCD 5
20
BCD 7
80
BCD 6
40
BCD 4
10
BCD0
1
BCD 3
8
BCD 2
4
BCD 1
2
Digital ground
+5V
Low
154
Agilent 1260 Infinity RID User Manual
CAN/LAN Cables
Identifying Cables 11
CAN/LAN Cables
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
Description CAN cable, Agilent module to module, 0.5 m CAN cable, Agilent module to module, 1 m
LAN Cables
p/n 5023-0203 5023-0202
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
Agilent Module to PC
p/n G1530-60600 RS232-61600
5181-1561
Description
RS-232 cable, 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, 8 m
156
Agilent 1260 Infinity RID User Manual
External Contact Cable
Identifying Cables 11
External Contact Cable
5
1
10
6
15
11
One end of this cable provides a 15-pin plug to be connected to Agilent modules interface board. The other end is for general purpose.
Agilent Module Interface Board to general purposes
External contact cable Agilent module interface board to general purposes (p/n G1103-61611)
Color
Pin Agilent module
Signal Name
White
1
Brown
2
Green
3
Yellow
4
Grey
5
Pink
6
Blue
7
Red
8
Black
9
Violet
10
Grey/pink
11
Red/blue
12
White/green 13
Brown/green 14
White/yellow 15
EXT 1 EXT 1 EXT 2 EXT 2 EXT 3 EXT 3 EXT 4 EXT 4 Not connected Not connected Not connected Not connected Not connected Not connected 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.
Agilent Technologies
159
12 Appendix
General Safety Information
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.
Indicates 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 and the user should not touch it when heated up.
WARNING
A WARNING alerts you to situations that could cause physical injury or death.
Do not proceed beyond a warning until you have fully understood and met the indicated conditions.
CAUTION
A CAUTION alerts you to situations that could cause loss of data, or damage of equipment.
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
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.
The operator of this instrument is advised to use the equipment in a manner as specified in this manual.
Safety Standards
This is a Safety Class I instrument (provided with terminal for protective earthing) and has been manufactured and tested according to international safety standards.
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
General Safety Information
Some adjustments described in the manual, are made with power supplied to the instrument, and protective covers removed. Energy available at many points may, if contacted, result in personal injury.
Any adjustment, maintenance, and repair of the opened instrument under voltage should be avoided whenever possible. When inevitable, this has to be carried out by a skilled person who is aware of the hazard involved. Do not attempt internal service or adjustment unless another person, capable of rendering first aid and resuscitation, is present. Do not replace components with power cable connected.
Do not operate the instrument in the presence of flammable 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.
162
Agilent 1260 Infinity RID User Manual
Appendix 12
The Waste Electrical and Electronic Equipment (WEEE) Directive (2002/96/EC)
The Waste Electrical and Electronic Equipment (WEEE) Directive (2002/96/EC)
NOTE
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.
This product complies with the WEEE Directive (2002/96/EC) marking requirements. The affixed label indicates that you must not discard this electrical/electronic product in domestic household waste.
Product Category: With reference to the equipment types in the WEEE Directive Annex I, this product is classed as a "Monitoring and Control 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 Information
WARNING
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.
Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries.
Replace only with the same or equivalent type recommended by the equipment manufacturer.
WARNING
Lithiumbatteri - Eksplosionsfare ved fejlagtig håndtering. Udskiftning må kun ske med batteri af samme fabrikat og type. Lever det brugte batteri tilbage til leverandøren.
WARNING
Lithiumbatteri - Eksplosionsfare. Ved udskiftning benyttes kun batteri som anbefalt av apparatfabrikanten. Brukt batteri returneres appararleverandoren.
NOTE
Bij dit apparaat zijn batterijen geleverd. Wanneer deze leeg zijn, moet u ze niet weggooien maar inleveren als KCA.
164
Agilent 1260 Infinity RID User Manual
Radio Interference
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
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) < 70 dB. · Sound Pressure Lp < 70 dB (A) · At Operator Position · Normal Operation · According to ISO 7779:1988/EN 27779/1991 (Type Test)
166
Agilent 1260 Infinity RID User Manual
Solvent Information
Appendix 12
Solvent Information
Flow Cell
To protect optimal functionality of your flow-cell: · Avoid the use of alkaline solutions (pH > 9.5) which can attack quartz and
thus impair the optical properties of the flow cell. · If the flow cell is transported while temperatures are below 5 °C, it must be
assured that the cell is filled with alcohol. · Aqueous solvents in the flow cell can built 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. · Brown glass ware can avoid growth of algae. · Small particles can permanently block capillaries and valves. Therefore
always filter solvents through 0.4 µm filters. · Avoid the use of the following steel-corrosive solvents:
· Solutions of alkali halides and their respective acids (for example, lithium iodide, potassium chloride, and so on),
· High concentrations of inorganic acids like 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: 2CHCl3 + O2 2COCl2 + 2HCl 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
Solvent Information
· 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 THF.
168
Agilent 1260 Infinity RID User Manual
Agilent Technologies on Internet
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
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
on internet 169 algae 167, 167 algea 135 ambient operating temperature 43 ambient non-operating temperature 43 analog signal 28 analog
cable 148 apg remote 29 ASTM
environmental conditions 42 automatic recycling after analysis 16 automatic zero before analysis 16 automatic purge 16
B
balance 91 baseline noise and drift 76 baseline noise 86 baseline
drift 86 equilibration 87
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
cautions 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
170
Agilent 1260 Infinity RID User Manual
Index
EMF (early maintenance feedback) 21 time since last purge 21
environment 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 lamp current too low 113 lamp current too high 112 lamp voltage too low 112 lamp voltage too high 112 leak sensor open 103 leak sensor short 103 leak 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 external contact cable 157
F
fan failed 105 features
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
H
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
I
installation bench space 42 delivery checklist 48 environment 42, 42, 42 flow connections 59
of in, waste and recycle capillaries 59 of the 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
Agilent 1260 Infinity RID User Manual
171
Index
lamp current too low 113 lamp voltage too high 112 lamp voltage too low 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
N
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
O
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 indicator 92 power consideration 40 power consumption 43 power cords 41
R
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 I 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 special settings
boot-resident 36 forced cold start 36 specification physical 43 specifications analog outputs 45 communications 45 GLP features 45 performance 44 safety and maintenance 45 stack configuration front view 52 rear view 55 status indicator 93 synchronization lost 102
T
temperature sensor 102 test chromatogram 126 tests
test chromatogram 126 timeout 100 troubleshooting
error messages 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
V
voltage range 43
W
wander 86 warnings and cautions 131 weight 43
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, · specifications, · installation, · configuration, · optimizing, · troubleshooting and diagnostics, · maintenance, · parts identification, · safety and related information.
Agilent Technologies 2010 , 2012
Printed in Germany 05/12
*G1362-90011* *G1362-90011*
G1362-90011 Rev. B
Agilent Technologies
Acrobat Distiller 10.1.3 (Windows)