Agilent Technologies 1100 Series User guide

s1
Agilent 1100 Series
Capillary LC System
System Manual

Notices
© Agilent Technologies, Inc. 2002
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
G1388-90001
Edition
08/2002
Printed in Germany
Agilent Technologies Deutschland GmbH
Hewlett-Packard-Strasse 8
76337 Waldbronn, Germany
ii
formance 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.
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.
Warning Symbols Used on the
Instrument
The apparatus is marked with this
symbol when the user should refer
to the instruction manual in order
to prevent risk of harm to the
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 per-
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.
!

iii
operator and to protect the
apparatus against damage.
1100 Series Capillary LC System
Manual
In This Manual…
This manual contains information for using your Capillary LC System.
1Installing your Capillary LC System
This chapter describes how to install and configure the Capillary LC
System.
2Optimizing Performance
This chapter discusses how to optimize your capillary LC system to
achieve best chromatographic results.
3Capillaries and Fittings
Overview of the capillaries and according fittings used in the capillary
LC System.
4Basic System Troubleshooting
This chapter includes examples of common problems and ways to feel
happy about them.
5Parts and Materials
Refer to this chapter for detailed illustrations and lists for identification
of parts and materials
6Options
In this chapter we will describe the different options available for the
capillary LC System.
7Specifications

Here you find performance specifications of the Capillary LC systems
Annex A Safety Information
1100 Series Capillary LC System Manual
iv 1100 Series Capillary LC System Manual

1100 Series Capillary LC System Manual v
Contents
1Installing your Capillary LC System
Site Requirements 2
Physical Specifications 4
System Installation Process 6
Installing a Capillary LC System with a Non-Thermostatted Sampler 7
Install the Diode Array Detector (DAD) (G1315B) 8
Install the Thermostatted Column Compartment (TCC) (G1316A) 9
Install the Micro Well-plate Sampler (G1377A) 10
Install the Capillary Pump (G1376A) 11
Install the Micro Vacuum Degasser (G1379A) 12
Install the Solvent Cabinet 13
Installing a Capillary LC System with a Thermostatted Micro Sampler 14
Install the Thermostat for 1100 Samplers (G1330B) 15
Install the Micro Sampler (G1387A Micro Autosampler (ALS), or G1378A
Micro Well-plate Sampler) 16
Install the Thermostatted Column Compartment (TCC) (G1316A) 17
Install the Diode Array Detector (DAD) (G1315B) 18
Install the Capillary Pump (G1376A) 19
Install the Micro Vacuum Degasser (G1379A) 20
Install the Solvent Cabinet 21
Get the System Ready for the First Injection 22
Manually Priming the Solvent Channels. 23
Purging the Pump24
Conditioning the System Under Method Conditions 25
Inject the Check-out Sample 26
Procedure 27

contents
vi 1100 Series Capillary LC System Manual
Typical Chromatogram 27
2Optimizing Performance
Hints for Successful Use of the Capillary Pump 30
Pump issues 30
Fused Silica Capillary issues 31
Sampler issues 32
Column thermostat issues
32 DAD issues 32
Solvent Information 33
Prevent Blocking of Solvent Inlet Filters 34
Checking the solvent inlet filters 34
Cleaning the Solvent Filters 35
Hints for the Micro Vacuum Degasser 36
When to use Alternative Seals 37
How to Choose the Primary Flow 38
Static Mixer and Filter 40
The standard static mixer 40 The
standard filter 40
How to Optimize the Compressibility Compensation Setting 41
The Fast Composition Change/Reconditioning Function 43
Purpose 43
How the Function Works 43
3Capillaries and Fittings
Capillary Flow Diagram 46
Connecting capillaries for the capillary LC system 47
Fittings and Ferrules 52
Instructions to connect a capillary. 53
Hints for Successful use of Capillaries and Fittings 54

1100 Series Capillary LC System Manual vii
contents
4Basic System Troubleshooting
System Pressure Abnormally Low
56
System Pressure Abnormally High 57
EMPV failed to initialize (micro mode only) 58
Unstable column flow and/or system pressure 59
Poor peak shape 61
Failure to produce peaks, or abnormally small peaks, after injection 62
Wandering Detector Baseline 63
User interface displays error messages for specific modules 64
5Parts and Materials
Micro Vacuum Degasser 66
Micro Vacuum Degasser Cover Parts 68
Capillary Pump 69
Solvent Cabinet and Bottle Head Assembly 71
Capillary Pump Hydraulic Path 72
Pump-Head Assembly 74
Capillary pump cover parts 76
Micro Well-plate Sampler 77
Sampling Unit for the Micro Well-plate Sampler 79
Micro Analytical Head Assembly 81
Micro Injection Valve Assembly 82
Micro Well-plate Sampler - Vial Trays
83

contents
viii 1100 Series Capillary LC System Manual
Micro Well-Plate Sampler Cover Parts
85
Thermostatted Micro Autosampler 86
Thermostat for 1100 Samplers 88
Sampling Unit for the Micro Autosampler 89
Micro Analytical Head Assembly 91
Micro Injection Valve Assembly 92
Thermostatted Micro Autosampler Cover Parts 93
Vial Trays94
Thermostatted Column Compartment 95
Micro Column Switching Valve 97
Thermostatted Column Compartment Sheet Metal Kit 98
Thermostatted Column Compartment Cover Parts99
Thermostatted Column Compartment Leak Parts 100
Diode Array Detector 101
DAD - Optical Unit Assembly 103
500 nl Flow Cell 105
Fan Assembly Parts 107
Holmium Oxide Filter 108
Diode Array Detector Cover Parts 109
Common Parts 110
Control Module (G1323B)110
Rear panel 111
Power and Status Light Pipes 112
Leak Parts 113
Foam parts 114
Sheet metal kit 114
Micro Degasser Accessory Kit 115
Capillary Pump Preventive Maintenance Kit G1376-68710 115

1100 Series Capillary LC System Manual ix
Capillary Pump Accessory Kit 116
Micro Well-plate Sampler Accessory Kit G1377-68705 117
Thermostatted Micro Autosampler Accessory Kit 118
Column Compartment with Micro Column Selection Valve Accessory Kit
119 DAD Accessory Kit 120
Cables 121
Analog Cables 123
Remote Cables 124
Agilent 1100 to 3396 Series II / 3395A Integrators 127
BCD Cables 130
Auxiliary Cable 132
contents
CAN Cable 132
External Contact Cable 133
RS-232 Cable Kit 134 LAN
Cables 134
6Options
Extended Flow Range Kit (G1376-69707) 136
Installing the Extended Flow Range Kit 138
0.1 - 2.5 ml/min Flow Capillary Kit (5065-4495) 139
Installing the 0.1 - 2.5 ml/min flow capillary kit 140
Micro Column Switching Valve G1388A#055 143
Parts Identification for Micro Column Switching Valve 145
Replacing Rotor Seal of Micro Column Switching Valve 146
Removing the Micro Column Switching Valve
147
Installing the Micro Column Switching Valve
150

contents
x 1100 Series Capillary LC System Manual
500 nl Flow Cell Kit G1315-68714 153
Special Information for Maintenance 154
Installation of the Flow Cell 156
Connecting Small I.D. Capillaries 160
Replacing or Cleaning Parts 161
7Performance Specifications
Performance Specifications Agilent 1100 Series Capillary Pump 166
Performance Specifications Agilent 1100 Series Micro Vacuum Degasser
168
Performance Specifications Agilent 1100 Series Thermostatted Micro
Autosampler 169
Performance specification Agilent 1100 Series Micro Well-plate Sampler
170
Performance Specifications Agilent 1100 Thermostatted Column
Compartment. 171
Performance Specifications Agilent 1100 Series DAD 172
A Safety Information
General 176
Operation 176
Safety Symbols 177
Lithium Batteries Information 178 Danish
Information: 178
Radio Interference 179
Sound Emission 179
Solvent Information 179
Agilent Technologies on Internet 180
Index 181

Agilent 1100 Series Capillary LC System
System Manual
1
Installing your Capillary LC System
Site Requirements 2
Physical Specifications 4
System Installation Process 6
Installing a Capillary LC System with a Non-Thermostatted Sampler 7
Installing a Capillary LC System with a Thermostatted Micro Sampler
14
Get the System Ready for the First Injection 22
Inject the Check-out Sample 26

1 Installing your Capillary LC System
2 1100 Series Capillary LC System Manual
Agilent Technologies 1
Site Requirements
A suitable environment is important to ensure optimum performance of the Capillary
LC system.
Power Consideration
The modules power supply has wide ranging capability (see Table 1 on page 4). It accepts
any line voltage in the range described in the above mentioned table. Consequently there
is no voltage selector in the rear of the modules. There are also no externally accessible
fuses, because automatic electronic fuses are implemented in the power supply.
To disconnect the modules from line, unplug the power cord. The power supply still uses some
power, even if the power switch on the front panel is turned off.
Shock hazard or damage of your instrumentation can result, if the devices are connected to a line
voltage higher than specified.
Power Cords
Different power cords are offered as options with the modules. The female end of each
of the power cords is identical. It plugs into the power-input socket at the rear of the
instruments. The male end of each of the power cords is different and designed to match
the wall socket of a particular country or region.
Never operate your instrumentation from a power outlet that has no ground
connection. Never use a power cord other than the power cord designed for your
region.
WARNING
WARNING
WARNING

Installing your Capillary LC System 1
1100 Series Capillary LC System Manual 3
Never use cables other than the ones supplied by Agilent Technologies to ensure proper
functionality and compliance with safety or EMC regulations.
Bench Space
The modules dimensions and weight (see Table 2 on page 5) allow to place the
Capillary LC system on almost any 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 the circulation of air and electric connections.
If a Thermostatted Well Plate Sampler is installed, an additional 25 cm (10 inches)
of space on either side for the circulation of air, and approximately 8 cm (3.1
inches) at the rear for electrical connections is required.
If a complete Agilent Capillary LC system is to be installed on the bench, make sure that
the bench is designed to carry the weight of all the modules. For a complete system
including the Thermostatted Well Plate Sampler it is recommended to position the
modules in two stacks. see “System Installation Process" on page 6.
Environment
Your modules will work within specifications at ambient temperatures and relative
humidity as described in Table 1 on page 4.
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
Agilent 1100 Series Capillary Pump" on page 166) 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.
Do not store, ship or use your modules under conditions where temperature
fluctuations could cause condensation within the modules. Condensation will damage
the system electronics. If your modules were shipped in cold weather, leave them in their boxes and
allow them to warm slowly to room temperature to avoid condensation.
Physical Specifications
WARNING
CAUTION

1 Installing your Capillary LC System
4 1100 Series Capillary LC System Manual
Table 1 Common Physical Specifications
Type
Specification
Comments
Line voltage
100 –120 or 220 –240 VAC, ± 10 %
Wide-ranging capability
Line frequency
50 or 60 Hz, ± 5 %
Ambient operating temperature
4 –55 °C (41 –131 °F)
Ambient non-operating temperature
-40 –70 °C (-4 –158 °F)
Humidity
< 95 %, at 25 –40 °C (77 –104 °F)
Non-condensing
Operating Altitude
Up to 2000 m (6500 ft)
Non-operating altitude
Up to 4600 m (14950 ft)
For storing the capillary
pump
Safety standards: IEC, CSA, UL
Installation Category II, Pollution Degree
2

Installing your Capillary LC System 1
1100 Series Capillary LC System Manual 5
1100
Table 2 Module Specific Specifications
Agilent 1100 Module
Part Number
Weight
Dimension (h × w × d)
Power
consumption
Capillary Pump
G1376A
17 kg
39 lb
345x435x180 (mm)
13.5x17x7 (inches )
220 VA max
Micro Vacuum Degasser
G1379A
7.5 kg
16.5 lb
345x435x80 (mm)
13.5x17x3.1 ( inches )
30 VA max
Thermostatted Micro Autosampler
(Micro-ALS)
G1387A
14.2 kg
31.3 lb
345x435X200 (mm)
13.5X17X8 (inches )
300 VA max
Micro Well-plate Sampler
(Micro-WPS)
G1377A/78A
15.5kg
34.2lb
200x345x435 (mm)
8 x13.5x17 (inches )
300 VA max
Thermostat Module
G1330A/B
18.5 kg
40.7 lb
345x435x144 (mm)
13.5X17X5.5 ( inches )
260 VA max
Thermostatted Column Compartment
(TCC)
G1316A
10.2 kg
22.5 lb
410x435x140 (mm)
16.1x17x5.5 ( inches )
320 VA max
Diode Array Detector (DAD)
G1315B
11.5 kg
26 lb
345x435x140 (mm)
13.5x17x5.5 ( inches )
220 VA max
System Installation Process
Damaged Packaging
If the delivery packaging shows signs of external damage, please call your sales and
service office immediately. Inform your service representative that something may have
been damaged during shipment.
If there are signs of damage, please do not attempt to install the damaged
module.
CAUTION

1 Installing your Capillary LC System
6 1100 Series Capillary LC System Manual
Installing a Capillary LC System with a Non-Thermostatted Sampler
These instructions will produce a single stack of modules, with the Diode Array
Detector (DAD) on the bottom. Required cables, tubes and capillaries for each module
are included with the system shipment, or found in the module accessory kits.
NOTE The Agilent part numbers for capillaries indicated in the text are intended for use with
the standard capillary pump, as the pump is shipped from the factory. If the optional
Extended Flow Range Kit (G1376-68707) is to be installed in the pump, several of
these capillaries, throughout the entire system, will be changed. Refer to chapter 6 for
detailed information on the Extended Flow Range Kit.
Refer to Chapter 3, “Capillaries and Fittings,” starting on page 45 for detailed
information on system plumbing connections, and Agilent part numbers and
descriptions for capillaries throughout the system.
This manual provides an overview of the entire Capillary LC System. For more detailed
information about each module, refer to the reference manual provided with each module.
Install the Diode Array Detector (DAD) (G1315B)
Ensure the line power switch at the fronto f the DAD is off. Connect the power cable to power only after you have finished the
hardware installation of all modules in the stack.
1Ensure the line power switch at the front of the Diode Array Detector ( DAD) is off.
2If the system is to be connected to the user interface by LAN, install the JetDirect
card into the DAD. See Replacing the Interface Board in the DAD Reference
Manual.
3Place the DAD on the bench.
4Connect one end of the LAN cross over cable (5183-4649) to the connector on the
JetDirect card. Connect the other end of the LAN cross over cable to the
Chemstation.
5Connect the Can-bus cable (5181-1516) to one of the CAN connectors at the rear of
the DAD.
WARNING

Installing your Capillary LC System 1
1100 Series Capillary LC System Manual 7
6Connect the power cable to the power socket at the rear of the DAD. Do not connect
the power cable to power until you have finished the hardware installation of all
modules in the stack.
7Install the DAD flow cell (G1314-68714).
8Route the DAD flow cell outlet capillary (G1315-68708) to an appropriate waste
container. The DAD flow cell inlet capillary (G1315-68703) will later be connected
to the outlet of the analytical column.
9Connect the large-bore corrugated plastic leak drain tubing to the DAD leak
drain fitting. Route the leak drain tubing to an appropriate waste container.
Install the Thermostatted Column Compartment (TCC) (G1316A)
Connect the power cable to power only after you have finished the hardware
installation of all modules in the stack.
1Ensure the line power switch at the front of the Thermostatted Column Compartment
(TCC) is off
2Place the TCC on top of the DAD. Make sure that the two modules are interlocked
correctly.
3Connect the Can-bus cable (5181-1516) to one of the CAN connectors at the rear of
the TCC.
4Connect the power cable to the power socket at the rear of the TCC. Do not connect
the power cable to power until you have finished the hardware installation of all
modules in the stack.
5Connect the free end of the Can-bus cable from the DAD to the unused Can-bus
connector at the rear of the TCC.
6Place the analytical column into the TCC. Observe the flow direction indicated on
the column. The column can later be secured using column clamp (5001-3702).
7Connect the DAD flow cell inlet capillary (G1315-68703) to the outlet of the
analytical column. NOTE Carefully route all capillaries so that they are not crushed
or broken by module front covers. Avoid excessive bending. Chapter 2 for advice on
handling capillaries.
WARNING

1 Installing your Capillary LC System
8 1100 Series Capillary LC System Manual
NOTE If your TCC has a Micro Column Switching Valve, refer to the Micro Column Switching Valve
information in Chapter 6 of this manual.

Installing your Capillary LC System 1
Connect the power cable to power only after you have finished the hardware
1100 Series Capillary LC System Manual 9
Install the Micro Well-plate Sampler (G1377A)
installation of all modules in the stack.
1Ensure the line power switch at the front of the micro well-plate sampler ( micro
WPS) is off.
2Place the micro WPS on top of the TCC. Make sure that the two modules are
interlocked correctly.
3Remove the sampler shipping protection foam.
4Connect the CAN-bus cable (5181-1519) to one of the CAN connectors at the rear
of the micro WPS.
5Connect the power cable to the power socket at the rear of the micro WPS. Do not
connect the power cable to power until you have finished the hardware installation
of all modules in the stack.
6Connect the free end of the Can-bus cable from the TCC to the unused Can-bus
connector at the rear of the micro sampler.
7Connect one end of the sampler-to-column capillary (G1375-87304) to port 6 of the
sampler injection valve. Connect the other end of this capillary to the inlet of the
WARNING

1 Installing your Capillary LC System
Connect the power cable to power only after you have finished the
hardware
10 1100 Series Capillary LC System Manual
analytical column in the TCC. NOTE Carefully route all capillaries so that they are
not crushed or broken by module front covers.
Avoid excessive bending. refer to Chapter 2 for advice on handling capillaries.
Install the Capillary Pump (G1376A)
installation of all modules in the stack.
1Ensure the line power switch at the front of the capillary pump is off.
2Place the capillary pump on top of the micro WPS. Make sure that the two modules
are interlocked correctly.
3Connect the power cable to the power socket at the rear of the capillary pump. Do
not connect the power cable to power until you have finished the hardware
installation of all modules in the stack.
4Connect the free end of the CAN-bus cable from the micro sampler to one of the
CAN-bus connectors at the rear of the capillary pump.
5Connect the pre-terminated end of the pump-to-sampler capillary (G1375-87310) to
the flow sensor outlet of the capillary pump. Connect the other end of this capillary
to port 1 of the sampler injection valve.
WARNING