Agilent 1100 Capillary LC System Manual
Agilent 1100 Capillary LC System Manual
Agilent 1100 Capillary LC System Manual
Capillary LC System
System Manual
s1
Notices
© Agilent Technologies, Inc. 2002 Warranty Safety Notices
No part of this manual may be reproduced in The material contained in this docu-
any form or by any means (including elec- ment is provided “as is,” and is sub-
tronic storage and retrieval or translation ject to being changed, without notice, CAU TI O N
into a foreign language) without prior agree- in future editions. Further, to the max-
ment and written consent from Agilent imum extent permitted by applicable A CAUTION notice denotes a hazard.
Technologies, Inc. as governed by United law, Agilent disclaims all warranties, It calls attention to an operating pro-
States and international copyright laws. either express or implied, with regard cedure, practice, or the like that, if
to this manual and any information not correctly performed or adhered
Manual Part Number contained herein, including but not
limited to the implied warranties of to, could result in damage to the
G1388-90001
merchantability and fitness for a par- product or loss of important data. Do
ticular purpose. Agilent shall not be not proceed beyond a CAUTION
liable for errors or for incidental or notice until the indicated conditions
Edition consequential damages in connec- are fully understood and met.
08/2002 tion with the furnishing, use, or per-
formance of this document or of any
Printed in Germany information contained herein. Should
Agilent Technologies Deutschland GmbH Agilent and the user have a separate WA RN ING
Hewlett-Packard-Strasse 8 written agreement with warranty
76337 Waldbronn, Germany terms covering the material in this
A WARNING notice denotes a haz-
document that conflict with these
terms, the warranty terms in the sep- ard. It calls attention to an operat-
arate agreement shall control. ing procedure, practice, or the like
that, if not correctly performed or
Technology Licenses adhered to, could result in personal
The hardware and/or software described in injury or death. Do not proceed
this document are furnished under a license beyond a WARNING notice until the
and may be used or copied only in accor- indicated conditions are fully
dance with the terms of such license.
understood and met.
!
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 operator
and to protect the apparatus against
damage.
2 Optimizing Performance
This chapter discusses how to optimize your capillary LC
system to achieve best chromatographic results.
6 Options
In this chapter we will describe the different options available
for the capillary LC System.
7 Specifications
Here you find performance specifications of the Capillary LC
systems
2 Optimizing 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
Vial Trays 94
Thermostatted Column Compartment 95
Micro Column Switching Valve 97
Thermostatted Column Compartment Sheet Metal Kit 98
Thermostatted Column Compartment Cover Parts 99
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
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
6 Options
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
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
7 Performance 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
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
Agilent Technologies 1
1 Installing your Capillary LC System
Site Requirements
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
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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
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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
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connection. Never use a power cord other than the power cord designed for your
region.
Never use cables other than the ones supplied by Agilent Technologies to ensure
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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
CAU TI O N
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
Non-operating altitude Up to 4600 m (14950 ft) For storing the capillary pump
1100
Diode Array Detector (DAD) G1315B 11.5 kg 345x435x140 (mm) 220 VA max
26 lb 13.5x17x5.5 (inches)
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.
CAU TI O N
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.
NO TE 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.
Connect the power cable to power only after you have finished the hardware
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installation of all modules in the stack.
1 Ensure the line power switch at the front of the Diode Array Detector
(DAD) is off.
2 If 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.
3 Place the DAD on the bench.
4 Connect 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.
5 Connect the Can-bus cable (5181-1516) to one of the CAN connectors at the
rear of the DAD.
6 Connect 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.
7 Install the DAD flow cell (G1314-68714).
8 Route 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.
9 Connect the large-bore corrugated plastic leak drain tubing to the DAD leak
drain fitting. Route the leak drain tubing to an appropriate waste container.
Connect the power cable to power only after you have finished the hardware
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installation of all modules in the stack.
1 Ensure the line power switch at the front of the Thermostatted Column
Compartment (TCC) is off
2 Place the TCC on top of the DAD. Make sure that the two modules are
interlocked correctly.
3 Connect the Can-bus cable (5181-1516) to one of the CAN connectors at the
rear of the TCC.
4 Connect 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.
5 Connect the free end of the Can-bus cable from the DAD to the unused
Can-bus connector at the rear of the TCC.
6 Place 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).
7 Connect the DAD flow cell inlet capillary (G1315-68703) to the outlet of the
analytical column.
NO TE 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.
NO TE If your TCC has a Micro Column Switching Valve, refer to the Micro Column Switching Valve
information in Chapter 6 of this manual.
Connect the power cable to power only after you have finished the hardware
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installation of all modules in the stack.
1 Ensure the line power switch at the front of the micro well-plate sampler
(micro WPS) is off.
2 Place the micro WPS on top of the TCC. Make sure that the two modules are
interlocked correctly.
3 Remove the sampler shipping protection foam.
4 Connect the CAN-bus cable (5181-1519) to one of the CAN connectors at the
rear of the micro WPS.
5 Connect 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.
6 Connect the free end of the Can-bus cable from the TCC to the unused
Can-bus connector at the rear of the micro sampler.
7 Connect 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 analytical column in the TCC.
NO TE 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.
Connect the power cable to power only after you have finished the hardware
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installation of all modules in the stack.
1 Ensure the line power switch at the front of the capillary pump is off.
2 Place the capillary pump on top of the micro WPS. Make sure that the two
modules are interlocked correctly.
3 Connect 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.
4 Connect 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.
5 Connect 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.
NO TE 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.
6 Connect the 1/8 inch plastic EMPV waste tube to the barbed waste fitting of
the EMPV. Route the waste tube to an appropriate waste container.
Connect the power cable to power only after you have finished the hardware
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installation of all modules in the stack.
1 Ensure the line power switch at the front of the micro vacuum degasser is
off.
2 Place the degasser on top of the pump. Make sure that the two modules are
interlocked correctly.
3 Connect one end of the remote cable (5061-3378) to the rear of the
degasser. Connect the other end of the cable to the remote port at the rear
of the pump.
4 The degasser accessory kit has a set of 4 solvent tubes (G1322-67300). Each
tube is labeled A, B, C or D. Connect each solvent tube to its intended
OUTLET channel port on the degasser.
5 Connect the other end of the solvent tube to its intended port at the pump
solvent selection valve. Follow the guide below:
These instructions will produce two stacks of modules. The left-hand stack
will consist of the capillary pump, degasser and solvent cabinet. The
right-hand stack will consist of the thermostatted micro sampler (bottom),
thermostatted column compartment (TCC), and diode array detector (DAD)
on top.
Required cables, tubes and capillaries for each module are included with the
system shipment, or found in the module accessory kits.
NO TE 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.
Connect the power cable to the thermostat module power socket only after you have
CAU TI O N
connected the thermostat-to-sampler cable (G1330-81600) between the thermostat
module and the micro sampler. Failure to follow this warning will result in damage to
the electronics of the thermostat module and the sampler.
1 Place the thermostat for 1100 samplers (thermostat module) on the bench.
The thermostat module should be no more than 25cm (9.8 inches) from the
front edge of the bench. The thermostat module should be positioned as the
bottom module in the right-hand stack.
2 Connect one end of the thermostat-to-sampler cable (G1330-81600) to the
26-pin connector at the rear of the thermostat module.
3 Route the large-bore plastic corrugated condensation drain tube from the
front of the thermostat module directly into an appropriate waste
container.
NO TE It is important that the condensation drain tube provides a straight, unblocked path for the
condensation to drain. The tube should never be coiled. The tube should never be below the
level of liquid in the waste container
Connect the power cable to the thermostat module power socket only after you have
CAU TI O N
connected the thermostat-to-sampler cable (G1330-81600) between the thermostat
module and the sampler. Failure to follow this warning will result in damage to the
electronics of the thermostat module and the sampler.
1 Ensure the line power switch at the front of the micro sampler is off.
2 Place the micro sampler on top of the thermostat module. Make sure that
the two modules are interlocked correctly.
3 Remove the sampler shipping protection foam.
4 Connect the free end of the thermostat-to-sampler cable (G1330-81600) to
the 26-pin connector at the rear of the micro sampler.
5 Connect the CAN-bus cable (5181-1519) to one of the CAN connectors at the
rear of the micro sampler.
6 Connect the power cable to the power socket at the rear of the micro
sampler. Connect the power cable to the power socket at the rear of the
thermostat module.
Do not connect these power cables to power until you have finished the
hardware installation of all modules in the stack.
7 Install the air channel adapter (G1329-43200) between the micro sampler
and the thermostat module. See the sampler reference manual for more
detail if required.
8 Connect one end of the sampler-to-column capillary (G1375-87304) to port
6 of the sampler injection valve. The other end of this capillary will later be
connected to the inlet of the analytical column in the TCC.
NO TE Carefully route all capillaries so that they are not crushed or broken by module front covers.
Avoid excessive bending. See Chapter 2 for advice on handling capillaries.
9 Connect the large-bore corrugated plastic leak drain tubing to the micro
sampler leak drain fitting. Route the leak drain tubing to an appropriate
waste container.
Connect the power cable to power only after you have finished the hardware
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installation of all modules in the stack.
1 Ensure that the line power switch at the front of the thermostatted column
compartment (TCC) is off.
2 Place the TCC on top of the micro sampler. Make sure that the two modules
are interlocked correctly.
3 Connect the Can-bus cable (5181-1516) to one of the CAN connectors at the
rear of the TCC.
4 Connect 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.
5 Connect the free end of the Can-bus cable from the micro sampler to the
unused Can-bus connector at the rear of the TCC.
6 Place 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).
7 Connect the free end of sampler-to-column capillary (G1375-87304) to the
inlet of the analytical column in the TCC.
NO TE Carefully route all capillaries so that they are not crushed or broken by module front covers.
Avoid excessive bending. See Chapter 2 for advice on handling capillaries.
Connect the power cable to power only after you have finished the hardware
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installation of all modules in the stack.
1 Ensure the line power switch at the front of the diode array detector DAD is
off.
2 If 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.
3 Place the DAD on top of the TCC. Make sure that the two modules are
interlocked correctly.
4 Connect 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.
5 Connect the free end of CAN-bus cable (5181-1516) from the TCC to one of
the CAN connectors at the rear of the DAD.
6 Connect 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.
7 Install the DAD flow cell (G1314-68714).
8 Route the DAD flow cell outlet capillary (G1315-68708) to an appropriate
waste container.
9 Connect The DAD flow cell inlet capillary (G1315-68703) to the outlet of the
analytical column.
Ccarefully route all capillaries so that they are not crushed or broken by module front covers. Avoid excessive bending. See chapter 2 for advice on handling capillaries.
NO TE Carefully route all capillaries so that they are not crushed or broken by module front covers.
Avoid excessive bending. See Chapter 2 for advice on handling capillaries.
Connect the power cable to power only after you have finished the hardware
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installation of all modules in the stack.
1 Ensure the line power switch at the front of the capillary pump is off.
2 Place the capillary pump on the bench, positioned to the left of the micro
sampler thermostat module.
3 Connect 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.
4 Connect the 1-meter CAN-bus cable (5181-1519) from one of the CAN-bus
connectors at the rear of the capillary pump to the free CAN-bus connector
at the rear of the micro sampler.
5 Connect the pre-terminated end of the pump-to-sampler capillary
(G1375-87310) to the flow sensor outlet of the pump. Connect the other end
of this capillary to port 1 of the micro sampler injection valve.
NO TE Carefully route all capillaries so that they are not crushed or broken by module front covers.
Avoid excessive bending. See Chapter 2 for advice on handling capillaries.
6 Connect the 1/8 inch plastic EMPV waste tube to the barbed waste fitting of
the EMPV. Route the waste tube to an appropriate waste container.
7 Connect the large-bore corrugated plastic leak drain tubing to the pump
leak drain fitting. Route the leak drain tubing to an appropriate waste
container.
Connect the power cable to power only after you have finished the hardware
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installation of all modules in the stack.
1 Ensure the line power switch at the front of the micro vacuum degasser
(degasser) is off.
2 Place the degasser on top of the pump. Make sure that the two modules are
interlocked correctly.
3 Connect one end of the remote cable (5061-3378) to the rear of the
degasser. Connect the other end of the cable to the remote port at the rear
of the pump.
4 The degasser accessory kit has a set of 4 solvent tubes (G1322-67300). Each
tube is labeled A, B, C or D. Connect each solvent tube to its intended
OUTLET channel port on the degasser.
5 Connect the other end of the solvent tube to its intended port at the pump
solvent selection valve. Follow the guide below:
When you are using the system for the first time after installation, best results
are obtained by performing the following 3-step system preparation, in the
order given below:
1 Manually priming the solvent channels.
2 Purging the pump.
3 Conditioning the system under method conditions.
When opening capillary or tube fittings, solvents may leak. Please observe
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appropriate safety precautions (such as eye protection, safety gloves, protective
clothing) as described in the material handling information and safety data sheet
supplied by the solvent vendor, especially when hazardous solvents are used.
NO TE This procedure should be done before the modules are turned on.
1 The degasser accessory kit contains a 20ml plastic syringe and a solvent
tube adapter for this syringe. Push the adapter onto the syringe.
2 Pour the intended analytical solvents into the solvent bottles, and install
the bottles on the desired solvent channels. Install Isopropanol on channels
which will not be used right away.
3 Put a paper towel over the leak sensor in the pump leak tray.
4 Disconnect the channel A solvent tube from the A1 port of the pump solvent
selection valve.
Liquid may drip from the disconnected solvent tube. Make sure to follow appropriate
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safety precautions.
5 Connect the end of the solvent tube to the syringe adapter. Slowly draw a
syringe volume (20ml) from the solvent tube.
6 Disconnect the solvent tube from the syringe adapter, and reconnect the
tube to the A1 port of the solvent selection valve. Eject the syringe contents
into an appropriate waste container.
7 Repeat steps 4 to 6 for the three remaining solvent channels.
8 When all 4 solvent channels are manually primed, remove the paper towel
from the pump leak tray. Make sure that the pump leak sensor is dry before
turning on the pump.
When the pump has been turned off for a certain time (for example, overnight), oxygen will re-diffuse into the channels between the degasser and the pump. It is suggested to purge each channel at 2500 ul/min for 1 minute at the beginning of each day.
NO TE When the pump has been turned off for a certain time (for example, overnight), oxygen will
re-diffuse into the channels between the degasser and the pump. It is suggested to purge
each channel at 2500 µl/min for 1 minute at the beginning of each day.
When switching between reverse Isopropanol Best solvent to flush air out of the
phase and normal phase (both system
times)
To clean the system when using Bidistilled water Best solvent to re-dissolve salts
buffers
The purpose of the instrument check is to demonstrate that all modules of the
instrument are correctly installed and connected. It is not a test of the
instrument performance.
A single injection of the Agilent Technologies isocratic test sample (Agilent
part number 01080-68704) is made under the method conditions given below:
For system configurations other than those shown above, the method
conditions might need to be altered to produce the desired chromatogram.
Procedure
1 Make a single injection of the isocratic test standard under the conditions
given Table 4 on page 26.
2 Compare the resulting chromatogram with the typical chromatogram
shown in Figure 1.
Typical Chromatogram
A typical chromatogram for this analysis is shown in Figure 1. The exact
profile of the chromatogram will depend on the chromatographic conditions.
Variations in solvent quality, column packing, standard concentration and
column temperature will all have a potential effect on peak retention and
response.
2
Optimizing Performance
Hints for Successful Use of the Capillary Pump 30
Solvent Information 33
Prevent Blocking of Solvent Inlet Filters 34
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
How to Optimize the Compressibility Compensation Setting 41
This chapter shows how to optimize your capillary LC system to achieve best
chromatographic results:
Agilent Technologies 29
2 Optimizing Performance
Pump issues
• Flush the pump extensively. First with in the purge mode, second with a
pressure applied to remove all the gas bubbles. It is recommended to do this
first with 100% A and than 100%B.
• The system pressure must be higher than 20 Bar at the pump outlet.
• In micro mode abnormally high column flow variations are an indication of
dirt within the system, blocked filters or loose pump valves.
• Place solvent cabinet with the solvent bottles always on top (or at a higher
level) of the capillary pump.
• Prevent blocking of solvent inlet filters (never use the pump without solvent
inlet filter). Growth of algae should be avoided.
• When using buffer solutions, flush the system with water before switching
it off.
• Check the pump plungers for scratches when changing the piston seals.
Scratched plungers will lead to micro leaks and will decrease the lifetime of
the seal.
• After changing the plunger seals, perform the seal wear-in procedure. See
the pump reference manual.
• Place the aqueous solvent on channel A and the organic solvent on
channel B. The default compressibility and flow sensor calibration settings
are set so. Always use the correct calibration values.
• For generation of fast gradients on short columns remove the mixer, enter
the new pump configuration and select the fast gradient range for the
primary flow rate (chromatographic performance will not be affected).
• When running the micro mode check the correct instrument setup (flow
sensor type, used mixer and filter).
• Make sure to observe the minimum recommended flow setpoint:
• Normal mode100 µl/min
• Micro mode, 20 µl flow sensor: 1 µl/min
• Micro mode, 100 µl flow sensor:10 µl/min
• To achieve the best flow stability, especially in the micro mode, %Ripple must
be within acceptable values, typically no worse than 2%.
NO TE Do not overtighten the fused silica capillaries. see Chapter 3, “Capillaries and Fittings,”
starting on page 45 for information on installing and handling capillaries.
• Be careful when you bend a Fused Silica Capillary. The diameter must not
be smaller than 40 mm.
40 mm
Sampler issues
• For fast gradient use valve to bypass function after the sample is transferred
to the column. This function results in smaller delay times and sharper
gradient curves.
• When doing automated gradient runs, use the fast composition
change/reconditioning function to equilibrate the system between runs.
DAD issues
• At very low flow rates, bubbles might form in the cell due to low pressure in
the cell. This might cause the detector signal to have spikes and noise.
Adding a 50 µm capillary to the outlet of the cell can reduce this effect.
• To avoid cell damage due to overpressure, set the upper pressure limit to
50 bar greater than the typical operating pressure.
Solvent Information
Always filter solvents through 0.4 µm filters, small particles can permanently
block the capillaries and valves. 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 and nitric acid,
especially at higher temperatures (replace, if your chromatography method
allows, 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.
• 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 dissolve stainless
steel.
• Avoid the use of alkaline solutions (pH > 8.5) which can attack the fused
silica from the capillaries.
Contaminated solvents or algae growth in the solvent bottle will reduce the
lifetime of the solvent filter and will influence the performance of the capillary
pump. This is especially true for aqueous solvents or phosphate buffers (pH 4
to 7). The following suggestions will prolong lifetime of the solvent filter and
will maintain the performance of the capillary pump.
• Use sterile, if possible amber, solvent bottles to slow down algae growth.
• Filter solvents through filters or membranes that remove algae.
• Exchange solvents every two days or refilter.
• If the application permits add 0.0001 to 0.001 Molar sodium acid to the
solvent.
• Place a layer of argon on top of your solvent.
• Avoid exposure of the solvent bottles to direct sunlight.
When opening capillary or tube fittings solvents may leak out. Please observe
WA RN ING
appropriate safety procedures (for example, goggles, safety gloves and protective
clothing) as described in the material handling and safety data sheet supplied by the
solvent vendor, especially when toxic or hazardous solvents are used.
The solvent filters are located on the low-pressure side of the capillary pump.
A blocked filter therefore does not affect the pressure readings of the capillary
pump. The pressure readings cannot be used to check whether the filter is
blocked or not. If the solvent cabinet is placed on top of the capillary pump,
the filter condition can be checked in the following way:
Remove the solvent inlet tube from the inlet port of the solvent selection valve
or the adapter at the active inlet valve. If the filter is in good condition the
solvent will freely drip out of the solvent tube (due to hydrostatic pressure). If
the solvent filter is partly blocked only very little solvent will drip out of the
solvent tube.
Never use the system without solvent filters. This could cause damage to the pump
CAU TI O N
valves
If you are using the vacuum degasser for the first time, if the vacuum degasser
was switched off for any length of time (for example, overnight), or if the
vacuum degasser lines are empty, you should prime the vacuum degasser
before running an analysis.
The vacuum degasser can be primed by pumping solvent with the capillary
pump at high flow rate (2.5 ml/min). Priming the degasser is recommended,
when:
• vacuum degasser is used for the first time, or vacuum chambers are empty.
• changing to solvent that are immiscible with the solvent currently in the
vacuum chambers.
• capillary pump was turned OFF for a length of time (for example during
night) and volatile solvent mixtures are used.
For more information see the Reference Manual for the Agilent 1100 series
micro vacuum degasser.
The standard seals for the capillary pump can be used for most applications.
However that use normal phase solvents (for example hexane) are not suitable
for the standard seals and require a different seal when used for a longer time
in the capillary pump. In this case we recommend the use of polypropylene
seals, part number 0905-1420 (pack of 2). These seals have less abrasion
compared to the standard seals.
Polyethylene seals have a limited pressure range 0-200 bar. When used above 200 bar
CAU TI O N
their lifetime will be significantly reduced. DO NOT apply the seal wear in procedures
performed with the standard seals at 400 bar.
Primary Flow is a parameter which exists only when the capillary pump is
used in the Micro mode. Primary flow is defined as the flow volume and
composition available at the inlet to the EMPV. Using this available primary
flow, the EMPV and flow sensor work together to deliver and control the
requested column flow. All primary flow in excess of the column flow is
delivered to waste via the 1/8 inch plastic waste tube connected to the EMPV
barbed waste fitting.
In every case, the pump automatically selects the best primary flow for the
requested column flow. This ensures optimum column flow stability under all
conditions. Primary flow selection is dependent on the current system
pressure, and on the existing pump configuration Therefore, it is important
that the pump configuration for filter volume and mixer volume is correct.
NO TE Primary flow always is much higher than column flow. This must be considered when
calculating the amount of solvent needed for unattended operation.
The user cannot request a specific primary flow value. However, one of three
available primary flow ranges can be selected by the user:
Actual primary flow values may vary from system to system. In any case the
standard configuration is changed, the primary flow could be higher
compared to the values in above table.
The capillary pump is equipped with a static mixer and an inline filter in front
of the EMPV.
NO TE Removing the mixer will result in an increase of the composition wander and higher
detector noise.
The compressibility compensation default settings are 50 × 10-6 /bar (best for
most aqueous solutions) for pump head A and 115 × 10-6 /bar (to suit organic
solvents) for pump head B. The settings represent average values for aqueous
solvents (A side) and organic solvents (B side). Therefore it is always
recommended to use the aqueous solvent on the A side of the pump and the
organic solvent on the B side. Under normal conditions the default settings
reduce the pressure pulsation to values (below 1 % of system pressure) that
will be sufficient for most applications. If the compressibility values for the
solvents used differ from the default settings, it is recommended to change the
compressibility values accordingly. Compressibility settings can be optimized
by using the values for various solvents described in Table 6 on page 42. If the
solvent in use is not listed in the compressibility table, when using premixed
solvents and if the default settings are not sufficient for your application the
following procedure can be used to optimize the compressibility settings:
NO TE Use the capillary pump in the Normal Mode at least 100 µl/min.
1 Start channel A of the capillary pump with the adequate flow rate. The
system pressure must be between 50 and 250 bar
2 Before starting the optimization procedure, the flow must be stable. Use
degassed solvent only. Check the tightness of the system with the pressure
test.
3 Your capillary pump must be connected to an Agilent ChemStation or an
Agilent 1100 control module, the pressure and%-ripple can be monitored
with one of these instruments,
otherwise connect a signal cable between the pressure output of the
capillary pump and a recording device (for example, 339X integrator) and
set parameters.
Zero 50 %
Att 2^3
Chart Speed 10 cm/min
4 Start the recording device with the plot mode.
Acetone 126
Acetonitrile 115
Benzene 95
Chloroform 100
Cyclohexane 118
Ethanol 114
Heptane 120
Hexane 150
Isobutanol 100
Isopropanol 100
Methanol 120
1-Propanol 100
Toluene 87
THF 95
Water 46
Purpose
The capillary pump and the micro well-plate sampler are recommended for
capillary LC applications. Capillary LC methods have very low column flow
rates, typically in the range of 1-20 µl/min. At such low flow rates,
re-equilibrating the system to the initial mobile phase composition between
automated gradient runs may require a long time. To conveniently
re-equilibrate the system between automated gradient runs, the Fast
Composition Change/Reconditioning function is implemented.
The Fast Composition Change/Reconditioning function is available only in a
system that includes both a capillary pump and a micro well-plate sampler.
This function can be set up to occur automatically between runs, and/or to
occur automatically after any manual composition change.
NOTE:
NO TE The high flow rate used for Fast System Flush is not user-defined. For the Fast System
Flush, the pump automatically sets a predetermined maximum pressure limit. This pressure
limit is determined by the hardware configuration of the pump.
The flow rate used for Fast System Flush is the highest flow which can be delivered
without exceeding the pressure limit.
2 When the Fast System Flush time has elapsed, the micro well-plate sampler
needle is returned to the needle-seat. The pump returns to the normal
operating mode, reconditioning the column at the flow and initial
composition defined in the current method. The column is reconditioned
for the Column Reconditioning time defined in the user interface.
If multiple injections are in progress, the next injection will begin when Fast
Composition Change/Reconditioning is completed.
3
Capillaries 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
Agilent Technologies 45
3 Capillaries and Fittings
SSV
EMPV
2
6 7 8
2
Mixer
3 3
Flow sensor
Damper
5
9
4
14
11 Column 10 13
Analytical
head
Flow cell Injection valve Needle
15
12 16
Waste Waste
Figure 2 Capillary flow diagram of the Agilent 1100 system capillary LC system
Refer to Table 8, Table 9 on page 48, Table 10, Table 11 on page 50, or Table 12
on page 50 for specific capillaries.
NO TE The pressure drops in Table 7 and Table 8 are calculated for water (viscosity 1) and for a
flow rate of 10 µl/min.
NO TE The pressure drops in Table 9 are calculated for water (viscosity 1) and for a flow rate of
50 µl/min.
Table 10 Specific capillaries for use with a flow higher than 200 µl/min
Descriptions 1 The capillary G1375-87400 connects the mixer and the manual purge valve.
to Table 10 2 The capillary G1375-87318 connects the manual purge valve and the injection valve (port1).
3 The capillary G1375-87312 connects the injection valve (port 6) and the heat exchanger (IN).
4 The capillary G1375-87306 connects between the injection valve (port 6) and the heat exchanger
(IN) if the thermostat G1330A/B is installed.
5 The capillary G1316-87300 connects between the heat exchanger (OUT) and the column.
NO TE The pressure drops in Table 10 are calculated for water (viscosity 1) and for a flow rate of
1000 µl/min.
Table 11 Specific capillaries for use with a micro CSV and a 20 µl flow sensor
Table 12 Specific capillaries for use with a micro CSV and a 100 µl flow sensor
NO TE The pressure drops in Table 11 and Table 12 are calculated for water (viscosity 1) and for a
flow rate of 10 µl/min.
Column 1 Column 2
3 2
4
5
6 1
To detector
NO TE The pressure drops in table 13 are calculated for water (viscosity 1) and for a flow rate of
10 µl/min.
NO TE The pressure drops in tables 7 to 13 are indicated values at a specific flow rate and with
water (viscosity = 1). For other solvents or other flow rates, use the indicated relation to
calculate the approximate pressure drop. Depending on tolerance of the capillary diameter
the pressure drop values can vary by +/- 25% compared to the calculated results.
Pressure (Bar) =
Flow(µl/min) x Viscosity (mPa*s) x Length(mm) x 21333 / 3.14 x Diameter4 (µm)
A Swagelock 1/16” SST fitting, front and back ferrule 10/pk 5062-2418
B Lite Touch 1/32” SST ferrule and lock ring 10/pk 5065-4423
D Finger Tight Double winged nuts and 1/32” ferrules 10/pk 5065-4422
NO TE The Lite Touch ferrule System may be used with any stainless steel nut, or corresponding
Lite Touch nut.
• Slide the nut, steel compression ring and PEEK ferrules, (in that order),
onto the tubing. The flattened end of the ring should face towards the nut
with the narrower end of the ferrule toward the ring.
• Insert into the receiving port. Hold the tubing to the bottom of the fitting
while tightening down the nut. Tighten comfortably finger-tight.
• Using a 4 mm wrench tighten the stainless steel nut down with a 1/4
wrench turn.
4
Basic 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
NO TE This troubleshooting guide deals with systemic problems of the capillary LC. For detailed
diagnostic, troubleshooting and repair information on specific LC modules (status
indicators, error messages, diagnostic tests, etc.), refer to the Reference Manual supplied
with the specific LC module.
Agilent Technologies 55
4 Basic System Troubleshooting
Symptoms:
The current system pressure is significantly below the typical system pressure
produced by this method with this column.
Leaks somewhere in the • Use a flashlight and absorbent tissue to search At very low flow rates, a leak may
system for leaks throughout the system. never accumulate enough liquid to
trigger the module leak sensors. Low
flow rate leaks are also very hard to
see.
Solvent channels are not • Perform a 2-minute purge at 2500 µl/min for This is especially likely if the system
correctly purged. %Ripple each solvent channel. has been unused for more than one
might also be too high day.
Dirty solvent inlet filters • Temporarily remove solvent inlet filters to see if To minimize this problem, prefilter
Solvent intake is being they are the cause of the problem. If so, clean or the mobile phase, and take
restricted, %Ripple might replace the solvent inlet filters. precautions against algae formation
also be too high in the water.
Symptoms:
The current system pressure is significantly above the typical system pressure
produced by this method with this column.
The analytical column has • Replace the column. Otherwise, backflush the
become plugged column or replace the column inlet frit.
The filter in front (upstream) • Perform a pump purge at 1000 µl/min using If a new filter does not reduce the
of the EMPV has become pure water. During the purge, check system pressure, replace the mixer.
plugged pressure. If pressure is >10 bar, replace the
EMPV filter.
A component in the • Using the sampler maintenance positions, For severe capillary tube plugs,
micro-sampler has become switch the sampler injection valve from acetone is a good backflushing
plugged. This could be the mainpass to bypass. If pressure is significantly solvent.
sample loop, needle, needle reduced:
seat assembly or injection a Backflush or change the needle seat assembly.
valve ports. b Replace the needle.
c Backflush or replace the sample loop capillary.
d Replace the injection valve rotor seal.
e Clean the stator head with acetone, and make
sure the stator head ports are free of particles.
Symptoms:
An attempt to pump in the micro mode has resulted in either an EMPV
Initialization Failed error message, or a permanent EMPV Initialization not
ready message.
The no-flow pressure of the • Set the flow to zero, and disconnect the blue This problem typically causes a
system is higher than 10 bar. flexible capillary going from the damper to the permanent EMPV Initialization not
mixer The system pressure reading should be ready message.
close to zero bar.
• If the system pressure reading is higher than 4
bar, call Agilent service, or refer to the Capillary
Pump Reference Manual.
The inlet to the EMPV has • Make sure the solvent channels are well purged. This problem typically causes an
been blocked, or partially • Check the EMPV filter. Perform a pump purge at EMPV Initialization Failed error
restricted. The EMPV cannot 1000 µl/min using pure water. During the purge, message
take in sufficient flow to check system pressure. If pressure is >10 bar,
deliver the correct flow replace the EMPV filter. If a new filter does not
output. The EMPV reduce the pressure, replace the mixer.
initialization routine cannot • Check the flow path from the damper outlet to
be done within the required the EMPV inlet for plugs or restrictions.
2-minute period. • Check the EMPV-to-flow sensor capillary for a
total plug or partial restriction. Replace the
capillary, or backflush the capillary with
acetone.
• Replace the EMPV assembly (G1361-60000).
Call Agilent service or refer to the Capillary
Pump Reference Manual.
Symptoms:
In the micro mode, the pump flow control system is active. The flow control
system continuously measures the actual value of column flow, and maintains
the requested column flow despite changes in system restriction. If the flow
control becomes defective, actual column flow, hence system pressure, will
fluctuate. If the system offers a changing restriction to the pump, actual
column flow will fluctuate as the pump tries to maintain flow against the
changing restriction. Therefore, in the micro mode, unstable column flow and
unstable system pressure usually appear together.
Unstable column flow and/or system pressure: Possible Causes and Suggested Actions
The flow setpoint is below the • Make sure that the column flow setpoint is Normal mode 100 µl/min
recommended minimum above the recommended minimum setpoint: Micro mode, 20 µl flow sensor
value. 1 µl/min
Micro mode, 100 µl flow sensor
10 µl/min
The system pressure is • Make sure that there is at least 20 bar pressure
insufficient for reliable flow being developed after the pump.
control (micro mode). • Add an additional capillary after the pump if
required.
Leaks somewhere in the • Use a flashlight and absorbent tissue to search At very low flow rates, a leak may
system. for leaks throughout the system. Check for leaks never accumulate enough liquid to
after the pump, and inside the pump (valves, trigger the module leak sensors. Low
fittings, etc.) flow rate leaks are also very hard to
• If operating in the micro mode, perform the see.
micro mode leak test. If operating in the normal Refer to the Capillary Pump
mode, perform the normal mode pressure test. Reference Manual for information on
these tests.
One or more solvent channels • Perform a 2-minute purge at 2500 µl/min for This is especially likely if the system
are not correctly purged. each solvent channel. has been unused for more than one
%Ripple might also be too day.
high.
Unstable column flow and/or system pressure: Possible Causes and Suggested Actions (continued)
Dirty solvent inlet filters. • Temporarily remove solvent inlet filters to see if To minimize this problem, prefilter
Solvent intake is being they are the cause of the problem. If so, clean or the mobile phase, and take
restricted. %Ripple might replace the solvent inlet filters. precautions against algae formation
also be too high. in the water.
Dirty EMPV (micro mode • Perform the EMPV cleaning procedure, followed
only) by the EMPV performance test. Refer to the
Capillary Pump Reference Manual.
Basic performance problems • Perform the pump Leak Test. Refer to the Capillary Pump
in the pump. Reference Manual for information on
the leak test.
Symptoms:
The peak shape has taken on a fronting or tailing characteristic.
Poorly made capillary • Using a flashlight and absorbent tissue, At very low flow rates, a leak may
connections, causing carefully check for leaks throughout the system, never accumulate enough liquid to
excessive dead volume or especially in the following areas: trigger the module leak sensors. Low
leaks in a a All micro-sampler valve ports. flow rate leaks are also very hard to
chromatographically b Column inlet and outlet. see.
significant area of the system c Flow cell inlet capillary, at the capillary/cell
body junction.
• Refer to chapter 3 for information on connecting
capillaries. Make sure the capillary connections
are correctly made throughout the system,
especially in the following areas:
a All micro-sampler valve ports.
b Column inlet and outlet.
c Flow cell inlet capillary, at the capillary/cell
body junction.
Capillaries which are • Refer to chapter 3 for advice on diagnosing an Capillaries which have been crushed
internally broken, especially internally broken capillary. Check capillaries for by module covers are often broken
those capillaries located in a an internal break, particularly the needle-seat internally, and may show no external
chromatographically capillary, the sampler valve-to-column capillary evidence of a break.
significant area. and the flow cell inlet capillary.
Symptoms:
There are no peaks, or the peak size is significantly below the typical peak size
for this method with this column.
Failure to produce peaks, or abnormally small peaks, after injection: Possible Causes and Suggested Actions
A leak in a sample carrying • Using a flashlight and absorbent tissue, At very low flow rates, a leak may
area of the system. carefully check for leaks in the following areas: never accumulate enough liquid to
a. All micro-sampler valve ports. trigger the module leak sensors. Low
b. The junction of the needle and sample loop flow rate leaks are also very hard to
capillary. see.
c. The needle/seat interface.
d. Column inlet and outlet.
e. Flow cell inlet capillary, at the capillary/cell
body junction.
The 40 µl chamber of the • In the user interface diagnostics, access the In most applications, only a small
micro-sampler metering head Change Piston function of the micro-sampler part of the available 40µl metering
has developed bubbles. maintenance positions. This function draws the head volume is used. At very low
metering piston fully inward, clearing the flows, bubbles may form in the
chamber. unused space between the metering
• Under flow conditions, activate this function for piston and the chamber wall. The
at least 5 minutes. The sampler valve must be in bubbles act to defeat the draw of
the mainpass position at this time. Any bubbles sample into the needle.
which have formed in the chamber will now be For best results in clearing bubbles,
cleared by the flow. the mobile phase being pumped
should not contain water.
Critical Decision Determine if the problem is in the DAD, or coming from the LC system:
Remove the flow cell from the DAD. Close the cell cover, and see if the baseline
performance improves.
1 If baseline performance has not improved:
a Replace the lamp(s).
b Evaluate the environment for excessive drafts, temperature changes, etc.
2 If baseline performance has improved, focus attention on the possible
causes and suggested actions below.
The analytical column • Bypass the column. Pump directly into the flow
cell. If performance improves, try a new column.
Running with the pump mixer • Reinstall the mixer, and evaluate the The mixer may have been removed in
removed performance of the baseline. If the baseline an attempt to reduce gradient delay
performance improves, a solution must be found volume.
which is a compromise between mixing volume
and other chromatographic requirements.
"Mixing Noise" when • Try premixing the mobile phase in one bottle, This problem occurs when one (or
pumping a binary mobile and pumping 100% from that one solvent both) of the solvents has a high
phase from two channels. channel. background absorbance at the
If baseline performance improves, a solution detection wavelength. In this case,
must be found which is a compromise between the pump’s mixing efficiency may
mixing volume and other chromatographic not be good enough to produce a
requirements. For an isocratic analysis, sufficiently homogeneous mobile
premixing and pumping 100% one channel is the phase.
best solution. The detector reacts to gluts of the
more detectable parts of the solvent
mixture, and baseline disturbances
result.
Unstable flow and/or system • Refer to the problem Unstable flow and/or Failure to maintain stable column
pressure. system pressure above. If your system suffers flow or system pressure can also
from this problem, go through the possible cause unwanted baseline activity.
causes and suggested actions described there.
User interface displays error messages for specific modules: Possible causes and suggested actions
A module has experienced a • Refer to the Reference Manual supplied with A specific error message for that
specific hardware failure the module. Follow the advice on module is displayed.
during operation troubleshooting and repair for the error message The status indicator of that module
displayed. is red.
5
Parts and Materials
Micro Vacuum Degasser 66,
Capillary Pump 69,
Micro Well-plate Sampler 77,
Thermostatted Micro Autosampler 86
Thermostatted Column Compartment 95,
Diode Array Detector 101,
Common Parts 110
Cables 121
This chapter shows detailed illustrations and lists for the parts identification
for the complete system. It is divided into module specific parts sections and a
common parts section.
Agilent Technologies 65
5 Parts and Materials
5 Fixing plate no PN
11
3
4
5
9
6
1 Cabinet kit, includes base, side panels, top and front cover 5062-8579
Capillary Pump
Table 18 gives an overview over the main assemblies of the capillary pump.
The item numbers refer to Figure 6:
14 1
13
2
12
11
10
9
3
8
4
6 5
1
2
3
8
4
7
5
6
1 Mixer G1312-87330
5 FS to inj valve cap (550 mm, 50 µm) for 20 µl flow sensor G1375-87310
FS to inj valve cap (550 mm, 100 µm) for 100 µl flow sensor G1375-87306
1
11
10 7
8
Figure 8 Capillary pump hydraulic path
Pump-Head Assembly
4* Apdater G1312-23201
1
2
3
11
4
10 5
9 6
7
8
Figure 9 Pump head assembly
1 Plastic cover kit (includes top, base and both sides) G1312-68703
13 1
12 2
11
14
10 5
9
6
8 7
16 1
3
15
14
5
13
9
10
12 11
1 Screws 0515-0850
3 Adapter 01078-23202
4
5
6
Note:
1
2
3
4
5
5 Spring G1313-09101
1
1
7
6 1
1
5
4
9
2,3
Description Rows Columns Plate height Volume (µI) Part Number Package
Cabinet kit, includes base, side panels, top and front cover 5065-4446
Light protection kit, includes dark front cover and side window 5064-8272
Fan 3160-1017
12 1
11 2
10 3
7 6
Figure 17 Thermostatted micro autosampler main assemblies
Figure 18 Thermostat
15 1
14 4
13
6
12
7
11 8
10 9
1 Screws 0515-0850
3 Adapter 01078-23202
4
5
6
1
2
3
4
5
4 Door repair kit (includes transparent side and front door) G1329-68707
5 Light protection kit (includes opaque side and front door, G1329-68708
opaque front cover)
Cabinet upgrade kit (includes side panels, top cover, transparent G1329-68706
side and front door, front cover and side insulation cover for
thermostatted autosampler)
3 4 5
Figure 22 Thermostatted micro autosampler cover parts
Vial Trays
5 Spring G1313-09101
9 Column switching valve, additional column switching valve parts, see 0101-1051
page 97
9 1
1 2
8 3
5
7 6
2 Stator ring No PN
4
6
Figure 26 Thermostatted column compartment sheet metal kit
5,7 Leak Kit, includes leak top and leak base G1316-68700
6
1
5
2
Table 42 gives an overview over the main assemblies of the diode array
detector:. The item numbers refer to Figure 29
9 Optical unit (exchange assembly), for additional optical unit parts, G1315-69002
see page 81
Fuse for BCD board, 250 mA (total of 4 are on the board) 2110-0004
9 1
8 2
7 3
12 Spring, for other holmium oxide filter parts, see page 108 1460-1510
16 Sealing G1315-47103
12
8
11
13
14 1
15
4
3
2
7
10 9
16
1
2
12 11
3, 4 3, 4
13
10
7 5
16 9
14 15 17 8
2 Fan 3160-1016
3 Spring 1460-1510
NO TE When the filter motor has been removed, the filter lever should not be reused. Use always a
new filter lever to assure correct fit on the filter motor shaft.
1
2
3
4
Common Parts
This chapter shows the parts identification of the common parts like rear
panel, power and status light pipes, leak parts, foam parts, sheet metal kit and
the different accessory kits. For cables see page 121.
Rear panel
1 4
Leak Parts
1 5
Foam parts
Syringe * 5062-8534
Seal 0905-1503
Filter 3150-0450
Tubing assembly no PN
Label halftray no PN
Fitting 5061-3303
Table 59 Column compartment with micro column selection valve (CSV) accessory kit
G1316-68725
Capillary column – detector 380 mm lg, 0.17 i.d. includes items 4, 5 and 6 (not G1315-87311
assembled)
Cables
Never use cables other than the ones supplied by Agilent Technologies to ensure
WA RN ING
proper functionality and compliance with safety or EMC regulations.
External contacts Agilent 1100 Series interface board to general purpose G1103-61611
LAN cable Twisted pair cross over LAN cable, 10 feet long 5183-4649
(for point to point connection)
Analog Cables
1 Shield Ground
2 Not connected
3 Center Signal +
4 Connected to pin 6
5 Shield Analog -
6 Connected to pin 4
7 Key
8 Not connected
1 Not connected
2 Shield Analog -
3 Center Analog +
1 Not connected
2 Black Analog -
3 Red Analog +
Remote Cables
NO TE START and STOP are connected via diodes to pin 3 of the 3394 connector.
Table 72 Agilent 1100 to HP 1090 LC, HP 1040 DAD or signal distribution module
BCD Cables
10 1 BCD 5 20
11 2 BCD 7 80
3 3 BCD 6 40
9 4 BCD 4 10
7 5 BCD0 1
5 6 BCD 3 8
12 7 BCD 2 4
6 - Key 4 8 BCD 1 2
1 9 Digital ground
2 15 +5V Low
1 1 BCD 5 20
2 2 BCD 7 80
3 3 BCD 6 40
4 4 BCD 4 10
5 5 BCD0 1
6 6 BCD 3 8
7 7 BCD 2 4
8 8 BCD 1 2
9 9 Digital ground
NC 15 +5V Low
Green 1 BCD 5 20
Violet 2 BCD 7 80
Blue 3 BCD 6 40
Yellow 4 BCD 4 10
Black 5 BCD0 1
Orange 6 BCD 3 8
Red 7 BCD 2 4
Brown 8 BCD 1 2
White 15 +5 Vt Low
Auxiliary Cable
Green 3
Yellow 4
Grey 5 DC + 5 V IN
Pink 6 Vent
CAN Cable
Both ends of this cable provide a modular plug to be connected to Agilent 1100
Series module’s CAN-bus connectors
One end of this cable provides a 15-pin plug to be connected to Agilent 1100
Series module’s interface board. The other end is for general purpose.
White 1 EXT 1
Brown 2 EXT 1
Green 3 EXT 2
Yellow 4 EXT 2
Grey 5 EXT 3
Pink 6 EXT 3
Blue 7 EXT 4
Red 8 EXT 4
Instrument PC
DCD 1 1 DCD
RX 2 2 RX
TX 3 3 TX
DTR 4 4 DTR
GND 5 5 GND
DSR 6 6 DSR
RTS 7 7 RTS
CTS 8 8 CTS
RI 9 9 RI
LAN Cables
Recommended Cables
For point to point connection (not using a network hub) use a twisted pair
cross over LAN cable (P/N 5183-4649, 10 feet long).
For standard network connections using a hub use category 5 UTP cables,
(P/N G1530-61480, 8 m long).
6
Options
Extended Flow Range Kit (G1376-69707) 136
0.1 - 2.5 ml/min Flow Capillary Kit (5065-4495) 139
Micro Column Switching Valve G1388A#055 143
500 nl Flow Cell Kit G1315-68714 153
This chapter describes the different options available for the capillary LC
System.
The extended flow range kit described in Table 80 lets you adapt your
capillary pump to enable it to work with flows up to 100 µl/min. In order to
decrease the system pressure when you increase the flow until 100 µl/min
some capillaries must be changed. These capillaries, (8, 9, 10, 11, 13) are
shaded in Figure 39 on page 137.
13 Capillary injection valve to analytical head (200 mm, 100 µm) G1375-87312
SSV
EMPV
Mixer
3 3
Flow sensor
Damper
5
9
4
14
11 Column 10 13
Analytical
head
Flow cell Injection valve Needle
15
12 16
Waste Waste
1 Using the 4 mm / 1/4 - 5/16 inch open wrenches disconnect the capillaries
8, 9, 10, 11 and 13. Refer to Figure 39 on page 137 to identify their location.
2 Remove the 20 µl flow sensor by unscrewing the 2 holding screws with the
2.5 mm hex key.
3 Install the 100 ul flow sensor and screw the 2 holding screws with the
2.5 mm hex key.
4 Using the 4 mm / 1/4 - 5/16 inch open wrenches connect the capillaries 8, 9,
10, 11 and 13 (refer to Figure 39 on page 137) to identify their location
NO TE If the pressure drop in the system is not to high you can leave the capillary G1375-68703
between the column and the detector (item 8). Otherwise change it as recommended with
the capillary G1375-87308.
NO TE To successfully install the capillaries and avoid the risk of a leak go to Chapter 3,
“Capillaries and Fittings.
It is possible to use the capillary pump with a flow rate higher than
100 µl/min. For this the pump must be used in the normal mode and some
hardware modifications are necessary.
From 100 to 200 µl/min, bypassing the electronic flow control is needed. No
other hardware modifications are necessary.
From 200 to 2500 µl/min bypassing the electronic flow sensor, installing the
manual purge valve (supplied with the accessory kit), changing the UV
detector cell and changing the capillaries in the flow path is needed.
The 0.1 to 2.5 ml/min flow capillary kit (5065-4495) include all the capillaries
needed to work with a flow from 200 to 2500 µl/min.
12 Replace the loop capillary with the capillary G1329-87302 if you have a
micro autosampler (G1389A) or with the capillary G1377-87300 if you have
a micro well-plate sampler (G1377/78A).
NO TE Don‘t forget to change the loop or syringe size to 40 µl in the injector configuration
windows of the user interface.
Needle seat assembly must be G1329-87101 with the 100 µm capillary (G1389A).
Needle seat assembly must be G1375-87317 with the 100 µm capillary ((G1377/78A).
13 Replace the capillary between the injection valve (port 6) and the column
with the capillary G1375-87312. If a thermostat (G1330A/B) is in place use
the capillary G1375-87306.
NO TE Above a flow of 200 µl/min it is recommend to rout the flow through the Peltier. The
capillary G1316-87300 is then connected between the Peltier “out” and the column inlet.
14 Replace the capillary between the column and the detector with the
capillary G1315-87311.
NO TE Replace the 500 nl flow cell with the standard flow cell (G1315-60012), the semi micro flow
cell (G1315-6001) or the high pressure flow cell (G1315-60015)
The pressures in Table 82 and Table 83 are indicated values, measured on one
system. These values can differ from one system to another.
Table 82 Pressure drop at 2.5 ml/min for different concentrations (no column)
% of organic phase Pressure (bar) for Methanol Pressure (bar) for Acetonitrile
0 165 162
20 170 169
40 158 154
60 132 128
80 100 95
100 75 72
Table 83 Pressure drop for different columns and different flow rates, with a gradient
from 0 to 100% Acetonitrile in 10 minutes.
The micro column switching valve allows to work with 2 columns and to select
either the one or the other. 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 40 shows the flow diagram when column 1 is active. Figure 41 shows
the flow diagram when column 2 is active.
From autosampler
Column 1 3 Column 2
2
4
5
1
6
To detector
From autosampler
Column 1 3 2 Column 2
4
5
6 1
To detector
The micro column switching valve allows also to work with a column
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.
From autosampler
Column 1 3 Column 2
2
4
5
1
6
To detector
3 Stator ring No PN
1 Remove capillaries from ports 1, 5, and 6. 2 Loosen each fixing stator screws two turns at a
time. Remove bolts from head.
Preparations for this procedure: 1 Disconnect the grounding connection of the valve
at the Z-panel.
• Turn off the column compartment.
• Disconnect the power cable.
• Disconnect capillaries.
• Remove column compartment from stack and place it
on the working bench.
• Remove the front cover, top cover and top foam
section.
2 Unscrew the Z-panel. 3 Press against the rear of the Z-panel to release the
metal plate from the guide and pull it carefully
upwards.
4 Lift the Z-panel together with the top plastic panel 5 Locate the ambient temperature sensor in the top
half-way out of the guide. plastic part and push it towards the rear.
6 Carefully remove the ambient temperature sensor 7 Pull the top plastic panel together with the Z-panel
plugged into the rear of the top plastic panel. completely out of the guide.
8 Remove the Valve from its location. For the installation refer to “Installing the Micro
Column Switching Valve" on page 150.
Preparations for this procedure are: 1 If no column switching valve was installed, remove
the RFI-shield and the plastic cover (no longer
• The column compartment is open as
used).
described in “Removing the Micro
Column Switching Valve" on page 147
3 Carefully insert the top plastic panel together with 4 Carefully plug the ambient temperature sensor into
the Z-panel into the guide and press it half-way the rear of the top plastic panel.
down.
Not e
Ensure that the ambient temperature sensor is completely plugged into the rear of the top plastic panel.
Ensure that during the next steps the flexible cables close to the heat exchanger assemblies are not
damaged.
5 Press the Z-panel together with the Top Plastic 6 Press down completely until it clicks into its
Panel completely down. holding position.
7 Fix the Z-panel with the two screws. 8 Reconnect the grounding connection of the valve at
the Z-panel.
9 Replace the foam section, the top cover and front cover.
10 Replace the column compartment into stack.
11 Reconnect capillaries.
12 Reconnect the power cable.
13 Turn on the column compartment.
This section describes the 500 nl flow cell for Agilent 1100 Series diode array
detector and multiple wavelength detector.
Features
• small dispersion through:
• 500 nl, 10 mm pathlength flow cell
• novel PEEK jacked quartz capillaries
(inlet 50 µm i.d., outlet 75 µm i.d.)
• novel “top sealing” fitting concept
• low RI sensitivity for flat baselines at low flow gradients with the use of an
optical reference wavelength
• good sensitivity through 10 mm pathlength and acceptable noise level
• the cartridge type concept allows customer specific capillary connections
up to the front end of the quartz cell
Performance Specification
Type Specification
Pathlength 10 mm
Volume 500 nl
The supplied PEEK capillaries for this flow cell have special surface treatment at both ends.
CAU TI O N DO NOT shorten the capillaries. This may cause leakage or damage.
Bending radius smaller than 10 mm may break the quartz capillary inside the PEEK
jacket. In this case high pressure may burst the PEEK jacket.
Always wear eye protection when working close to polymer tubing that is under
CAU TI O N
pressure.
Do not use PEEK tubing with tetrahydrofuran (THF) or concentrated nitric acid (except
for short flushing procedures) and sulfuric acid.
Methylene chloride and dimethyl sulfoxide cause PEEK to swell.
During assembling take care for cleanliness.
The capillary may be reused by carefully removing of the ferrules using a pair
of side-cutters or the original Upchurch tool, see Figure 45.
The cell fittings are factory installed and tested for leakage. These connections
should not be used as an instrument interface. It should be opened only for
maintenance and/or special adaptions.
Do not overtighten the cell fittings. This may break the cell quartz body.
CAU TI O N
With the instrument accessory kit comes a 4-mm wrench and with the Sealing
Kit a special adapter. Both together work as a torque wrench with pre-defined
torque (maximum allowed torque for the cell fittings is 0.7 Nm). It can be used
to tighten the capillary fittings at the flow cell body. The wrench has to be
plugged into the adapter as shown in Figure 46.
Adapter
Wrench
max
0.7 Nm
1 Disconnect the capillaries from the capillary holder 2 Insert the union “Top Adjust” (supplied with the kit)
and remove the flow cell. into the lower capillary holder position. This will be
used as tool for fixing the ferrules at the capillaries.
Step 3 and 4 have to be done for each of the two flow 3 Slide the screw, back ferrule and front ferrule onto
cell capillaries, if this connection type is desired. the PEEK capillary (see detail for correct direction).
This is for cell side only!
There is no stop within the union “Top Seal” for plane
capillaries. Therefore one prefixed ferrule is required front
at least. ferrule
back ferrule
screw
4 Carefully press the capillary into the adjustment 5 Appearance of the prefixed ferrule.
union. Then tight the fitting screw moderately to fix
the ferrule.
~ 0.3 mm clearance
NO TE
Note:
6 The figure below shows the sealing principle within Depending on the fitting type you select, the figure in
the union “top seal”, hand tightened before torque is step 7 may look different.
applied.
The figures in step 7 and 8 show alternatively the
supplied PEEK fittings and the two supplied (top
sealing) unions from the kit (the original union(s)
must be replaced).
The figure in step 9 shows the connection with the
supplied SST fittings.
union top seal
capillaries touch
each other
7 Insert the flow cell into the instrument and connect 8 Insert the PEEK capillaries from the flow cell body
the waste and column capillary. together with the PEEK fitting into the supplied
unions and tighten it.
IN IN
OUT OUT
9 Insert the PEEK capillaries from the flow cell body Remove the flow cell and perform a leak test.
together with the SST fitting, ferrule and cone into
If no leak is observed, install the flow cell and you are
the union and tighten it.
ready to work.
NO TE A PEEK sleeve with the appropriate internal and outer diameter is required to fit the SST
fitting and the ferrules on the quartz capillary.
insert
The quartz block can be cleaned with alcohol. DO NOT touch the inlet and outlet
CAU TI O N
windows at the quartz block.
1 Disconnect the capillaries from the capillary holder 2 Unscrew the cell body from the holder.
and remove the flow cell.
3 Unscrew the capillaries from the flow cell. DO NOT 4 Using a toothpick, press on the plastic part and slide
use the adapter at this time! the quartz body out of the cell housing.
5 The quartz body and the cell seal assembly can be 6 This figure shows the correct holding of the quartz
separated for cleaning purpose. body and the cell seal assembly.
7 Replace the cell seal assembly onto the quartz body. 8 Slide the quartz body completely into the cell body to
It is recommended to use a new assembly. the front stop (use for example a toothpick).
9 Insert the flow cell capillaries and tighten them 10 Reassemble the flow cell body to the holder.
fingertight.Use of the wrench and torque adapter as
described page 155 and tighten the fittings alternate
11 Re-install the flow cell and connect the capillaries to Remove the flow cell and perform a leak test.
the union holder.
If no leak is observed, install the flow cell and you are
ready to work.
IN
OUT
7
Performance 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
Type Specification
System delay volume Typically 5 µl from EFC to column head, for flow rates up to 20 µl/min
(default setup).
Typically 14 µl from EFC to column head, for flow rates up to 100 µl/min
(default setup).
Type Specification
Hydraulic system Two dual piston in series, with proprietary servo-controlled variable
stroke drive, floating piston, active inlet valve, solvent selection valve
and electronic flow control for flow rates up to 100 µl/min
Column flow precision < 0.7 % RSD or 0.03 % SD (typically 0.4 % RSD or 0.02 % SD), at
10 µl/min and 50 µl/min column flow (based on RT, default setting)
Optimum composition 1 to 99% or 5 µl/min per channel (primary flow), whatever is greater
range
Composition precision < 0.2 % SD, at 10 µl/min (20 µl flow sensor), 50 µl/min (100 µl flow
sensor) and 1 ml/min (normal mode) default setting
Type Specification
Delay volume Typically 3 µl from the electronic flow control to the pump outlet for flow
rates up to 20 µl/min.
Typically 12 µl from the electronic flow control to the pump outlet for
flow rates up to 100 µl.
for flow rates up to 100 µl/min and electronic flow control active:
primary flow path 180 - 480 µl without mixer, 600 - 900 µl with mixer
(system pressure dependant)
Typically 180 to 480 µl (system pressure dependent) without mixer for
flow rates up to 2.5 ml/min. (Mixer delay volume 420 µl)
Recommended pH 1.0 – 8.5, solvents with pH < 2.3 should not contain acids which attack
range stainless steel. Upper pH range is limited by fused silica capillaries.
Safety and maintenance Extensive diagnostics, error detection and display (through control
module and Agilent ChemStation), leak detection, safe leak handling,
leak output signal for shutdown of pumping system. Low voltages in
major maintenance areas.
Type Specification
Number of channels 4
pH range 1 – 14
Evaporation of solvents into the < 200 µg/m3 Acetonitrile and Methanol
atmosphere certification by IAS.
Type Specification
Sample capacity 100 x 2 ml vials in 1 tray. Microvials (100 or 300 µl) with sleeves
(reduced cooling performance with microvials)
Recommended pH-range 1.0 – 8.5, solvents with pH < 2.3 should not contain acids which
attack stainless steel. Upper pH range is limited by fused silica
capillaries.
Material in contact with Stainless steel, sapphire, PTFE, PEEK, fused silica, Vespel
solvent
Safety features Leak detection and safe leak handling, low voltages in
maintenance areas, error detection and display
Type Specification
Safety features Leak detection and safe leak handling, low voltages in maintenance
areas, error detection and display
Injection range 0.01 – 8 µl in 0.01 µl increments with the small loop capillary
0.01 – 40 µl in 0.01 µl increments with the extended loop capillary
Type Specification
Short term noise Typically ± 3 × 10-5 AU at 254 nm at flow For the 500 nl flow cell the
(ASTM)* rates <100 µl/min noise is 2-3 times higher
Single and than with standard flow
Multi-Wavelength cell
* ASTM: “Standard Practice for Variable Wavelength Photometric Detectors Used in Liquid Chroma-
tography”.
For specification on the 500 nl flow cell refer to Table 85 on page 153.
A
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.
General
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 fuseholders must be avoided.
Any adjustment, maintenance, and repair of the opened instrument under voltage is
WA RN ING
forbidden.
Disconnect the instrument from the line and unplug the power cord before
WA RN ING
maintenance.
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.
Safety Symbols
Table 93 shows safety symbols used on the instrument and in the manuals.
Symbol Description
The apparatus is marked with this symbol when the user should refer to the instruction manual in
order to protect the apparatus against damage.
Eye damage may result from directly viewing the light produced by the deuterium lamp used in this
product. Always turn off the deuterium lamp before opening the metal lamp door on the side of the
instrument.
A warning alerts you to situations that could cause physical injury or damage to the
WA RN ING
equipment. Do not proceed beyond a warning until you have fully understood and
met the indicated conditions.
A caution alerts you to situations that could cause a possible loss of data. Do not
CAU TI O N
proceed beyond a caution until you have fully understood and met the indicated
conditions.
Danger of explosion if battery is incorrectly replaced. Replace only with the same or
WA RN ING
equivalent type recommended by the equipment manufacturer. Lithium batteries
may not be disposed-off into the domestic waste.
Danish Information:
NO TE Bij dit apparaat zijn batterijen geleverd. Wanneer deze leeg zijn, moet u ze niet weggooien
maar inleveren als KCA
Radio Interference
Never use cables other than the ones supplied by Agilent Technologies to
ensure proper functionality and compliance with safety or EMC regulations.
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)
Solvent Information
Observe the following recommendations on the use of solvents.
Solvents
Brown glass ware can avoid growth of algae.
Always filter solvents, small particles can permanently block the capillaries.
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).
system pressure
high, 57
low, 56
unstable, 59
system troubleshooting, 55
T
TCC
installing, 9
temperature
range, 171
stability, 171
temperature, ambient, 3
thermostatted capillary LC system
installing, 14
troubleshooting, 55
U
unpacking the pump, 4
V
voltage range, 4
W
warm-up time, 171
wavelength
accuracy and bunching, 172
range, DAD, 172
'
%%(&'
'
%%(&'
G1388-90001