Agilent Technologies 1200 series User manual

A
Agilent 1200 Series
Thermostatted Column
Compartment
G1316A /G1316B
User Manual

2 1200 Series TCC User Manual
Notices
© Agilent Technologies, Inc. 2006
No part of this manual may be reproduced in
any form or by any means (including elec-
tronic storage and retrieval or translation
into a foreign language) without prior agree-
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States and international copyright laws.
Manual Part Number
G1316-90010
Edition
Edition 02/06
Printed in Germany
Agilent Technologies
Hewlett-Packard-Strasse 8
76337 Waldbronn, Germany
Manual Structure
The User Manual G1316-90010 (English)
and its localized versions contain a subset
of the Service Manual and is shipped with
the Thermostatted Column Compartment in
printed matter.
Latest versions of the manuals can be
obtained from the Agilent web.
The Service Manual G1316-90110 (English)
contains the complete information about
the Agilent 1200 Series Thermostatted Col-
umn Compartment. It is available as Adobe
Reader file (PDF) only.
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1200 Series TCC User Manual 3
In This Guide…
This manual covers the Agilent 1200 Series Thermostatted
Column Compartments (TCC)
1Introduction to the Column Compartment 9
This chapter gives an introduction to the TCC, instrument
overview and internal connectors.
2Site Requirements and Specifications 25
This chapter gives information on environmental requirements,
physical and performance specifications.
3Installing the Column Compartment 31
This chapter describes the installation of the TCC.
4How to optimize the Column Compartment 43
This chapter gives hints on how to optimize the TCC.
5Troubleshooting and Diagnostics 45
Overview about the troubleshooting and diagnostic features.
6Test Functions 51
This chapter describes the TCC’s built in test functions.
7Maintenance and Repairing 59
This chapter provides general information on maintenance and
repair of the TCC.
8Maintenance 65
This chapter describes the maintenance of the TCC.
G1316A Agilent 1200 Series TCC
G1316B Agilent 1200 Series TCC-SL

4 1200 Series TCC User Manual
9Parts and Materials for Maintenance 75
This chapter provides information on parts for maintenance.
AAppendix 95
This chapter provides addition information on safety, legal and
web.

1200 Series TCC User Manual 5
Contents
1 Introduction to the Column Compartment 9
Introduction to the Column Compartment 10
Extendended Specifications on G1316B SL 11
System Overview 13
Column-Identification System 15
Column-Identification Tag 17
Column Clip 18
Column Switching Valve (Optional) 19
Electrical Connections 21
Instrument Layout 23
2 Site Requirements and Specifications 25
Site Requirements 26
Physical Specifications 28
Performance Specifications 29
3 Installing the Column Compartment 31
Unpacking the Column Compartment 32
Optimizing the Stack Configuration 33
Installing the Column Compartment 36
Flow Connections of the Column Compartment 39
Installation of Heater and Cooling Devices 42

6 1200 Series TCC User Manual
Contents
4 How to optimize the Column Compartment 43
Optimizing the Column Compartment 44
Using Additional Heater and Cooling Devices 44
5 Troubleshooting and Diagnostics 45
Overview of the Column Department’s Indicators and Test Functions 46
Status indicators 47
Power Supply Indicator 47
Instrument Status Indicator 48
User Interfaces 49
Agilent LC Diagnostic Software 50
6TestFunctions51
Thermostat Function Test 52
Temperature Calibration 54
Temperature Calibration Procedure 55
Calibration Problems 56
Installing the Temperature Sensor 57
7 Maintenance and Repairing 59
Introduction to Maintenance and Repair 60
Warnings and Cautions 61
Cleaning the Column Compartment 62
Using the ESD Strap 63
8 Maintenance 65
Overview of Maintenance 66
Changing Column Identification Tags 67
Replacing Head Parts of Column Switching Valve 69

Contents
1200 Series TCC User Manual 7
Adding Heater and Cooling Devices (G1316B SL) 71
Correcting Leaks 73
Replacing the Column Compartment’s Firmware 74
9 Parts and Materials for Maintenance 75
Valve Options Overview 76
Heater and Cooling Devices for G1316B 77
Column Switching Valve 2 Position/6 Port 79
Micro Column Switching Valve 2 Postion/6 Port 81
Micro Column Switching Valve 2 Position/10 Port 82
Accessory Kits 85
G1316A Accessory Kit (Standard) 85
G1316A Accessory Kit (2PS/10PT modules) 86
G1316B SL Accessory Kit (Standard) 87
G1316B SL Capillary System Kit 88
G1316B SL Micro Valve Kit 2 Position/10 Port 89
Column Regeneration Kit 90
Plastic Parts 92
Leak Parts 93
A Appendix 95
General Safety Information 96
Lithium Batteries Information 99
Radio Interference 100
Sound Emission 101
Solvent Information 102
Agilent Technologies on Internet 104

8 1200 Series TCC User Manual
Contents
Index 105

9
Agilent 1200 Series Thermostatted Column Compartment
User Manual
Agilent Technologies
1
Introduction to the Column
Compartment
Introduction to the Column Compartment 10
Extendended Specifications on G1316B SL 11
System Overview 13
Column-Identification System 15
Column Switching Valve (Optional) 19
Electrical Connections 21
Instrument Layout 23
This chapter gives an introduction to the TCC, instrument overview and
internal connectors.

10 1200 Series TCC User Manual
1 Introduction to the Column Compartment
Introduction to the Column Compartment
The Agilent 1200 Series thermostatted column compartment is a stackable
temperature-controlled column compartment for LC. It is available as
standalone module or as a component of a Agilent 1200 Series system. It is
used for heating and cooling to meet extreme requirements of retention time
reproducibility.
The main features of this column compartment are:
•Peltier heating and cooling from 10 degrees below ambient up to 80 °C
(G1316A) or 100 °C (G1316B SL) 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,
•to reduce the risk of additional dispersion, for low flow rates additional
heating and cooling devices were implemented (G1316B SL),
•to reduce the delay volume, a kit has been set up for installing a small
heat-exchangers with 1.6 µl delay volume and also a new cooling device
with 1.5 µl is available (G1316B SL),
•electronic column-identification module as standard for GLP
documentation of column type, and major column parameters,
•optional high-quality Rheodyne®column switching valve with ceramic
stator-face assemblies for prolonged lifetime.
For specifications, see “Performance Specifications” on page 29.

1200 Series TCC User Manual 11
Introduction to the Column Compartment 1
Extendended Specifications on G1316B SL
The 1200 series G1316B SL thermostatted column compartment is usable from
10°C below ambient up to 80° for flow ranges up to 5 ml/min and up to 100°C
for flow ranges up to 2.5 ml/min. To reduce the risk of additional dispersion
for low flow rates additional heater and cooling devices were implemented,
see Figure 1. The additional parts can be installed in any position in the
column compartment, see also “Installation of Heater and Cooling Devices” on
page 42.
The standard column compartment is equipped with a 3 µl and 6 µl heater or
cooler. Both can be set at the same or different temperature. To reduce the
delay volume, a kit (see “G1316B SL Capillary System Kit” on page 88) has
been set up for installing a small heaters with 1.6 µl internal delay volume and
also a new cooling device with 1.5 µl internal volume is available.
Figure 1 New additional heater and cooling devices
L-shaped pre-column heater
Volume: 1.6 µl
mounted on carrier
U-shaped Post-column cooler
Volume: 1.5 µl
mounted on Carrier
L-shaped pre-column
heater (Heater
long-up)
L-shaped pre-column
heater (Heater
long-down)

12 1200 Series TCC User Manual
1 Introduction to the Column Compartment
NOTE If the additional heater and cooling devices are used as shown in Figure 1, the column
identification system cannot be used. If the column identification system is required, fix the
heater and cooling devices in the upper or lower locations or fix them right/left of the
current location.
NOTE The use and optimization of the new small heat-exchangers and cooling devices is
described in detail in a Technical Note.

1200 Series TCC User Manual 13
Introduction to the Column Compartment 1
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 surface of the heat exchanger is shaped such that the area around
the column is kept on similar temperature level as the liquid running through
the column. This is done by thermal convection and radiation between the
heat exchanger fins. With this design it is ensured 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.
For example, temperature setpoint is 40 °C. The heat-exchanger temperature
is controlled at 40.8 °C and at the column entry there could be 39.8 °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).
NOTE Default mode: heater actual, column ± offset
Corrected mode: heater ± offset, column actual

14 1200 Series TCC User Manual
1 Introduction to the Column Compartment
Figure 2 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 are settable from the user interface). However this does
not mean that the column is at the correct temperature. The equilibration of
the column can take longer. Stability of the high pressure readings is a good
indication for equilibrium.
The temperature calibration and verification is described in the Service
Manual.
Figure 2 Equilibration of Heat Exchanger and Column Temperature
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17
20
25
30
35
40
45
Time (min)
Temperature (°C)
Column temperature
Heat exchanger temperature
Example for a flow rate of 5 ml/min of water

1200 Series TCC User Manual 15
Introduction to the Column Compartment 1
Column-Identification System
The Agilent 1200 Series thermostatted column compartment is equipped with
a column-identification system. This allows to write and to read
column-specific information to and from the column-identification tag.
Figure 3 Column-Identification System
Column-identification
tag, see page 17
Colum Clip, see page 18
Antennas

16 1200 Series TCC User Manual
1 Introduction to the Column Compartment
Table 1 shows the information that can be stored. The information fields can
be edited via the user interface.
The number of injections will be updated each run to create a column lifecycle
(history). The user interface allows to edit all information.
Table 1 Column-Identification Module Information
Item Example Comment
Product number 79916OD-552
Serial number 950522 Date of manufacturing
Batch number 1675
Geometry [mm] 100 × 2.1
Stationary phase ODS Hypersil
Particle size 10 µm
Number of injections 1267 See Note below.
Maximum pressure allowed [bar] 400
Maximum temperature recommended [°C] 70
Maximum pH recommended 12
Column void volume [ml]
NOTE If a column switching valve (see page 19) is installed in the module, the update of the
number of injections depends on the position of the column switching valve. For example, if
the left column is selected, the right column is not updated, and vice versa.
If no column switching valve is installed both sides are updated at the same time.

1200 Series TCC User Manual 17
Introduction to the Column Compartment 1
Column-Identification Tag
When correctly placed on the heat exchanger, the distance between tag and
antenna is 1–2 mm. This is the optimum distance for proper function. The
identification tag can be easily removed from the column.
NOTE For small diameter columns, a cable tie wrap should be used, to fix the
column-identification tag at the column (in case you modify your own column). Assure that
the tie wrap is not blocking the front cover.
NOTE There is a difference in attaching the identification tag to the column depending on which
heat exchanger it will be located, see Figure 4 on page 17 and Figure 5 on page 17. The
Agilent logo should be always at the front side.
Figure 4 Column-Identification Tag for Left Heat Exchanger
Figure 5 Column-Identification Tag for Right Heat Exchanger
Column-identification tag
Column-identification tag

18 1200 Series TCC User Manual
1 Introduction to the Column Compartment
Column Clip
For better positioning of the column on the heat exchanger a column clip is
available (see “Accessory Kits” on page 85).
Figure 6 Column Clip (part number 5063-6526, pack of 6)

1200 Series TCC User Manual 19
Introduction to the Column Compartment 1
Column Switching Valve (Optional)
Two Column Selection
The valve can select either column 1 or column 2. The offline column is sealed
by connecting head to rail. Switching should be done when the flow is off and
the pressure is zero.
Figure 7 Location of Column Switching Valve
Figure 8 Column 1 Active
1
2
3
4
6
To detector
From autosampler
Column 1 Column 2
Heater assembly 1 Heater assembly 2

20 1200 Series TCC User Manual
1 Introduction to the Column Compartment
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.
Figure 9 Column 2 Active
Figure 10 Precolumn Back-flushing
1
2
3
4
6
To detector
From autosampler
Column 1 Column 2
Heater assembly 1 Heater assembly 2
1
2
3
4
6
From autosampler
Precolumn
Analytical
Column
Heater assembly 1 Heater assembly 2
To detector