Agilent Technologies 1290 infinity User manual

Agilent Technologies
Agilent 1290 Infinity
Thermostatted Column
Compartment
User Manual

1290 Infinity TCC User Manual
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Manual Part Number
G1316-90030
Edition
07/10
Printed in Germany
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1290 Infinity TCC User Manual 3
In This Guide...
In This Guide...
This manual covers the Agilent 1290 Infinity Thermostatted Column
Compartment (TCC) (G1316C).
1 Introduction to the Column Compartment
This chapter gives an introduction to the TCC, instrument overview and
internal connectors.
2 Site Requirements and Specifications
This chapter provides information on environmental requirements, physical
and performance specifications.
3 Installing the Module
This chapter provides information on unpacking, checking on completeness,
stack considerations and installation of the module.
4 How to optimize the Column Compartment
This chapter provides information on how to optimize the Thermostatted
Column Compartment.
5 Troubleshooting and Diagnostics
Overview about the troubleshooting and diagnostic features.
6 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.
7 Test Functions and Calibrations
This chapter describes the TCC’s built in test functions.

4 1290 Infinity TCC User Manual
In This Guide...
8 Maintenance
This chapter describes the maintenance tasks for the TCC. If the instrument
needs repair please contact your Agilent service representative.
9 Parts and Materials for Maintenance
This chapter provides information on parts for maintenance.
10 Identifying Cables
This chapter summarizes information on all cables.
11 Appendix
This chapter provides addition information on safety, legal and web.

1290 Infinity TCC User Manual 5
Contents
Contents
1 Introduction to the Column Compartment 9
Overview of the Module 10
System Overview 11
Column-Identification System 13
Column Switching Valve (Optional) 15
Early Maintenance Feedback 24
Instrument Layout 25
Electrical Connections 26
Interfaces 29
Setting the 8-bit Configuration Switch 34
2 Site Requirements and Specifications 41
Site Requirements 42
Physical Specifications 45
Performance Specifications 46
Extended Specifications on G1316C 47
3 Installing the Module 49
Unpacking the module 50
Optimizing the Stack Configuration 51
Installing the Column Compartment 56
Installing Valve Heads 61
Installation of Heater Devices 64
Flow Connections of the Column Compartment 66
Placing Columns 74
4 How to optimize the Column Compartment 77
Optimizing the Column Compartment 78
Using Additional Heater Devices 79
Delay Volume and Extra-Column Volume 80
How to Configure the Optimum Delay Volume 82
How to Achieve Higher Injection Volumes 83
How to Achieve High Throughput 84

6 1290 Infinity TCC User Manual
Contents
5 Troubleshooting and Diagnostics 87
Overview of the Module’s Indicators and Test Functions 88
Status indicators 89
Available Tests vs User Interfaces 91
Agilent Lab Advisor Software 92
6 Error Information 93
What Are Error Messages 94
General Error Messages 95
TCC Error Messages 100
7 Test Functions and Calibrations 111
Thermostat Function Test 112
Pressure Test 114
Temperature Calibration 115
8 Maintenance 119
Introduction to Maintenance and Repair 120
Cautions and Warnings 121
Overview of Maintenance 123
Cleaning the Column Compartment 124
Changing Column Identification Tags 125
Adding Heater Devices 127
Installing the capillaries 131
Correcting Leaks 141
Replacing Valve Heads 142
Preparing the Thermostatted Column Compartment for Transportation 145
Replacing the Module Firmware 147
9 Parts and Materials for Maintenance 149
Valve Options Overview 150
Heater and Cooling Devices 152
Column Switching Valve 8 Position-9 Port 155
2 pos/6 Port Ultra High Pressure Valve Head 156
2Pos/10Port Ultra High Pressure Valve Head 157
8Pos/9Port Ultra High Pressure Valve Head 158

1290 Infinity TCC User Manual 7
Contents
2pos/6 port valve head 600 bar 159
2pos/10 port valve head 600 bar 160
8pos/9 port valve head 600 bar 161
Accessory Kits 162
10 Identifying Cables 167
Cable Overview 168
Analog cables 170
Remote Cables 172
BCD Cables 175
CAN Cable 177
RS-232 Cable Kit 178
Agilent Module to Printer 179
11 Appendix 181
General Safety Information 182
The Waste Electrical and Electronic Equipment (WEEE) Directive
(2002-96-EC) 185
Lithium Batteries Information 186
Radio Interference 187
Sound Emission 188
Solvent Information 189
Agilent Technologies on Internet 190

8 1290 Infinity TCC User Manual
Contents

9
1290 Infinity TCC User Manual
Agilent Technologies
1
Introduction to the Column
Compartment
Overview of the Module 10
System Overview 11
Column-Identification System 13
Column Switching Valve (Optional) 15
Typical Applications 18
Early Maintenance Feedback 24
Instrument Layout 25
Electrical Connections 26
Serial Number Information 27
Rear view of the module 28
Interfaces 29
Overview Interfaces 30
Setting the 8-bit Configuration Switch 34
Communication Settings for RS-232C 37
Special Settings 39
This chapter gives an introduction to the TCC, instrument overview and internal
connectors.

10 1290 Infinity TCC User Manual
1Introduction to the Column Compartment
Overview of the Module
Overview of the Module
The Agilent 1290 Infinity thermostatted column compartments is a stackable
temperature-controlled column compartment for LC. It is available as
standalone module or as a component of an Agilent 1290 Infinity system. It is
used for heating and cooling to meet extreme requirements of retention time
reproducibility.
The main features of the 1290 Infinity thermostatted column compartment
are:
•Peltier heating and cooling from 10 degrees below ambient up to 100 °C
with high heating and cooling speeds for maximum application flexibility
and stability,
•holds up to three 30 cm columns and optimized design gives minimum dead
volumes and maximum efficiency,
•two independently programmable heat exchangers contribute volumes of
only 3 and 6 µl,
•additional heating devices for low flow rates, which reduce the risk of
additional dispersion,
•it can be supplemented by a kit to install a small heat-exchanger with 1.6 µl
delay volume to reduce the delay volume.
•electronic column-identification module as standard for GLP
documentation of column type, and major column parameters,
•optional high-quality Rheodyne®column switching valves with ceramic
stator-face assemblies for prolonged lifetime.
For specifications, see “Performance Specifications” on page 46.

1290 Infinity TCC User Manual 11
Introduction to the Column Compartment 1
System Overview
System Overview
The Concept of Heating and Cooling
The design of this thermostatted column compartment uses column heating
and cooling devices with Peltier elements. The solvent entering the column
compartment is heated up or cooled down to a settable temperature with two
low-volume heat exchangers (3 µl on left side, 6 µl on right side), made of a
short piece of capillary 0.17 mm i.d. leading through a heat exchanger. The
heat exchanger is designed such that it can function simultaneously as an air
heater. The shape of the heat exchanger surface allows the area around the
column to be kept at a similar temperature level as the liquid running through
the column. This is done by thermal convection and radiation between the
heat exchanger fins. This design ensures that the column and the solvent
flowing through it are almost at the same temperature.
Actual temperature control is accomplished at the heat exchanger. The solvent
cools down or heats up on its transfer from the heating block to the column
inlet. This depends on several factors: flow rate, setpoint temperature,
ambient temperature and column dimensions.
In a flow-through temperature regulation system, there are necessarily slightly
different temperatures at different positions. If, for example, the temperature
set by the user is 40 °C, then the heat exchanger is regulated to a temperature
40.8 °C which is different by a certain offset (here 0.8 °C). The solvent
temperature at the column entry would be about 39 °C.
The actual temperature displayed on the user interface is always the derived
temperature taken at the heat exchanger, corrected by the offset explained
above.
Any type of heated column compartment brings one important consequence
for column temperature equilibration. Before an equilibrium is reached, the
whole mass of column, column packing, and solvent volume inside the column
has to be brought to the selected temperature. This depends on several factors:
flow rate, setpoint temperature, ambient temperature and column dimensions.
The higher the flow rate, the faster the column equilibrates (due to
thermostatted mobile phase).

12 1290 Infinity TCC User Manual
1Introduction to the Column Compartment
System Overview
“Temperature Calibration” on page 115 shows a setpoint temperature of 40 °C.
Some time after entering the setpoint the heat exchanger has reached its
temperature and the control activity starts. The TEMPERATURE NOT READY
signal will be cancelled 20 seconds after the sensed temperature was within a
range of ± 0.5 °C of the setpoint (other values can be set via the user
interface). However this does not necessarily mean that the column has
already reached the correct temperature. The equilibration of the column may
take longer. Stability of the pressure signal is a good indication for
equilibrium.
Figure 1 Equilibration of Heat Exchanger and Column Temperature
The temperature calibration and verification is described in the Service
Manual.
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1290 Infinity TCC User Manual 13
Introduction to the Column Compartment 1
Column-Identification System
Column-Identification System
The Agilent 1290 Infinity thermostatted column compartment is equipped
with a column-identification system. It allows to read and write
column-specific information to and from the column-identification tag.
Figure 2 Column-Identification System
Table 1 on page 14 shows the information that can be stored. The information
fields can be edited via the user interface.
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14 1290 Infinity TCC User Manual
1Introduction to the Column Compartment
Column-Identification System
The number of injections will be updated each run to create a column lifecycle
(history). The user interface allows to edit all information.
If a 2 Position/6 Port valve and 2 Position/10 Port valve (see “Column
Switching Valve (Optional)” on page 15) is installed in the module, the update
of the number of injections depends on the position of the column switching
valve. If the valve connects the left column to the flow path, the left but not the
right column tag is updated (and vice versa). If no column switching valve is
installed, both sides are updated at the same time. If an 8 Position/9 Port valve
is installed, no tag is updated for avoiding ambiguity as more than 2 columns
might be installed.
Tab le 1 Column-Identification Module Information
Item Example Comment
Product number 79916OD-552
Serial number 950522 Date of manufacturing
Batch number 1675
Geometry 100 mm × 2.1 mm
Stationary phase ODS Hypersil
Particle size 10 µm
Number of injections 1267 See below.
Maximum pressure allowed 400 bar
Maximum temperature recommended 70 °C
Maximum pH recommended 12
Column void volume

1290 Infinity TCC User Manual 15
Introduction to the Column Compartment 1
Column Switching Valve (Optional)
Column Switching Valve (Optional)
Figure 3 Location of Column Switching Valve
Two Column Selection
The valve can select either column 1 or column 2. The offline column is sealed
by connecting head to tail. Switching should be done when the flow is off and
the pressure is zero.
NOTE Before switching the valve, switch off the pump or set the flow to zero. Keeping the flow on
while the valve is switched can cause exceeding the maximum pressure. This will stop
method or sequence execution.

16 1290 Infinity TCC User Manual
1Introduction to the Column Compartment
Column Switching Valve (Optional)
Figure 4 Column 1 Active
Figure 5 Column 2 Active
Precolumn Back-flushing
The sample is injected into series-connected precolumn and analytical
column. After the valve has switched, the analytical column flow continues in
normal direction. Only the precolumn is back-flushed, eluting highly retained
peaks directly to the detector.
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1290 Infinity TCC User Manual 17
Introduction to the Column Compartment 1
Column Switching Valve (Optional)
Figure 6 Precolumn Back-flushing
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18 1290 Infinity TCC User Manual
1Introduction to the Column Compartment
Column Switching Valve (Optional)
Typical Applications
Dual column selection
2pos/6port valve (p/n G4231A/B) and 2pos/10port valve (p/n G4232A/B)
Advantages:
•Increase productivity
•Higher instrument up-time
Quickly change between two different stationary phases to check your
separation selectivity, or use two identical stationary phases to have the
second column immediately available after the first one loses efficiency, for
example with complex matrices.
Sample enrichment and sample cleanup
2pos/6port valve (p/n G4231A/B) and 2pos/10port valve (p/n G4232A/B)
Advantages:
•Easy automation of sample preparation
•Higher reproducibility
•Increased productivity and sensitivity
Sample cleanup is essential for samples with complex matrices, such as
biological fluids, food extracts and waste water. Before injection into a LC or
LC/MS system, the sample matrix must be separated from the analytes of
interest. Otherwise, contaminants can disrupt separation and detection or
even damage the analytical column.

1290 Infinity TCC User Manual 19
Introduction to the Column Compartment 1
Column Switching Valve (Optional)
Figure 7 Sample enrichment

20 1290 Infinity TCC User Manual
1Introduction to the Column Compartment
Column Switching Valve (Optional)
Figure 8 Sample clean-up