Analytical SFC System Service Manual
Analytical SFC System Service Manual
Service Manual
Agilent Technologies
Notices
Agilent Technologies, Inc. 2010 - 2012 Warranty receive no greater than Restricted Rights as
defined in FAR 52.227-19(c)(1-2) (June
No part of this manual may be reproduced
The material contained in this docu- 1987). U.S. Government users will receive
in any form or by any means (including elec-
ment is provided as is, and is sub- no greater than Limited Rights as defined in
tronic storage and retrieval or translation
into a foreign language) without prior agree-
ject to being changed, without notice, FAR 52.227-14 (June 1987) or DFAR
ment and written consent from Agilent in future editions. Further, to the max- 252.227-7015 (b)(2) (November 1995), as
Technologies, Inc. as governed by United imum extent permitted by applicable applicable in any technical data.
States and international copyright laws. law, Agilent disclaims all warranties,
either express or implied, with regard Safety Notices
Manual Part Number to this manual and any information
contained herein, including but not CAUTION
G4301-90100 Rev. C limited to the implied warranties of
merchantability and fitness for a par- A CAUTION notice denotes a
Edition ticular purpose. Agilent shall not be hazard. It calls attention to an
05/2012 liable for errors or for incidental or
consequential damages in connection
operating procedure, practice, or
Printed in Germany the like that, if not correctly per-
with the furnishing, use, or perfor-
Agilent Technologies mance of this document or of any formed or adhered to, could
Hewlett-Packard-Strasse 8 information contained herein. Should result in damage to the product
76337 Waldbronn Agilent and the user have a separate
written agreement with warranty
or loss of important data. Do not
This product may be used as a com-
ponent of an in vitro diagnostic sys- terms covering the material in this proceed beyond a CAUTION
tem if the system is registered with document that conflict with these notice until the indicated condi-
the appropriate authorities and com- terms, the warranty terms in the sep- tions are fully understood and
plies with the relevant regulations. arate agreement shall control.
met.
Otherwise, it is intended only for gen-
eral laboratory use. Technology Licenses
The hardware and/or software described in WA R N I N G
this document are furnished under a license
SFC Fusion and Aurora SFC Fusion are and may be used or copied only in accor- A WARNING notice denotes a
trademarks of Aurora SFC Systems, Inc. All dance with the terms of such license. hazard. It calls attention to an
rights reserved.
Restricted Rights Legend operating procedure, practice,
The Agilent 1260 Infinity Analytical SFC
System includes a special designed Agilent If software is for use in the performance of a
or the like that, if not correctly
1260 Infinity system including a G4301 A U.S. Government prime contract or subcon- performed or adhered to, could
Aurora SFC Fusion A5 module. tract, Software is delivered and licensed as result in personal injury or
Commercial computer software as
defined in DFAR 252.227-7014 (June 1995),
death. Do not proceed beyond a
or as a commercial item as defined in FAR WARNING notice until the indi-
2.101(a) or as Restricted computer soft- cated conditions are fully under-
ware as defined in FAR 52.227-19 (June
1987) or any equivalent agency regulation stood and met.
or contract clause. Use, duplication or dis-
closure of Software is subject to Agilent
Technologies standard commercial license
terms, and non-DOD Departments and
Agencies of the U.S. Government will
In This Book
8 Identifying Cables
This chapter provides information on cables used with the Agilent 1200
Infinity Series modules.
9 Appendix
This chapter provides addition information on safety, legal and web.
Contents
9 Appendix 129
General Safety Information 130
The Waste Electrical and Electronic Equipment (WEEE) Directive
(2002/96/EC) 133
Radio Interference 134
Sound Emission 135
Solvent Information 136
Agilent Technologies on Internet 137
1
Introduction to Supercritical Fluid
Chromatography (SFC)
History of SFC 8
Theory of SFC 9
Benefits of SFC 10
Common flow path overview for packed column SFC instrumentation 11
The Agilent 1260 Infinity Analytical SFC System 12
The SFC Fusion A5 (G4301A) 13
HPLC-SFC binary pump (G4302A) 13
SFC-Autosampler (G4303A) 14
The Column Compartment (G1316C) 14
UV-detection (DAD G1315C and MWD G1365C) 15
Applications 15
Columns 16
This chapter provides an overview of the history, theory and benefits of SFC.
Agilent Technologies 7
1 Introduction to Supercritical Fluid Chromatography (SFC)
History of SFC
History of SFC
Theory of SFC
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Figure 1 State of a solvent
Benefits of SFC
SFC is widely accepted for the analysis and separation of chiral compounds. In
addition, it gains increasing acceptance as a complementary liquid-based
separation technique to HPLC for high-throughput and high-resolution
analysis of complex mixtures. This is due to the thermodynamic properties of
supercritical fluids, which can be exploited for high throughput and high
efficiency. In addition, the mild thermal conditions also allow for the analysis
of thermally labile compounds. Typically, analysis times and column
re-equilibration are decreased by a factor of 35 compared to standard HPLC.
With the increasing costs of organic solvents and the environmental
awareness to minimize toxic waste, production SFC is increasingly accepted
as the green alternative to normal phase or reversed phase chromatography,
gaining popularity in method development and UV- and MS-based separation
and purification. A variety of parameters, such as stationary phase selection,
mobile phase composition, modifier type and concentration, column
temperature and system pressure, can be easily manipulated to fulfill
separation requirements by influencing, optimizing and exploiting selectivity
in SFC.
The Agilent 1260 Infinity Analytical SFC System (G4309A) consists of a binary
HPLC-SFC pump (G4302A), a degasser (G1322A), an SFC Autosampler
(G4303A), a thermostatted column compartment (G1316C), and either a DAD
(G1315C) or MWD (G1365C) equipped with a high pressure SFC flow cell and
the SFC Fusion A5 module (G4301A). The SFC Fusion A5 module,
redestills and preconditions the CO2 by boosting the pressure to just below the
column head pressure, relieving the HPLC-SFC pump of any compression
requirements. This results in low detector noise and significantly higher
sensitivity. Therefore, the Agilent HPLC-SFC pump receives pre-conditioned
CO2, and acts only as metering device for the mobile phase flow and to form
the gradient with the second pump head by adding the appropriate amount of
modifier solvent. Downstream of the detector, the mobile phase is redirected
back into the SFC Fusion A5 to an integrated back pressure regulator that
maintains the backpressure over the system. The Agilent 1260 Infinity SFC
system with the Aurora SFC Fusion A5 module is completely controlled by
Agilent ChemStation software. The system diagram is shown below:
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SFC-Autosampler (G4303A)
In SFC, the complete solvent flow path needs to be pressurized under all
conditions to avoid expansion of the supercritical fluid. This excludes the use
of a variable injection loop design that is generally used in other Agilent
autosamplers. Therefore, the autosampler used in the Agilent 1260 Infinity
analytical SFC system has been converted to a fixed loop injector containing a
5 L sample loop.
The injection loop of the autosampler is installed between two ports of the 2
position/6 port injection valve. The total delay volume of the injector is about
3.3 L. As with any fixed loop injector, overfill of sample is necessary to inject
5 L reproducibly. To completely fill the sample loop, an excess of sample is
required. This is about 3 loop volumes (15 L of the installed loop) of sample
to achieve 95 % of the maximum loop volume. For smaller injection volumes,
the loop needs to be partially filled by sandwiching the sample between two
air bubbles, one on either side, followed by a plug of modifier or other solvent
behind the sample. Default methods for full loop filling are provided, and
should be used as initial injection conditions. The default methods are
automatically loaded in ChemStation.
Applications
SFC has gained a wide interest and acceptance in many small molecule
applications because of its high separation speed and efficiency, selectivity,
low operating costs, and due to low generation of organic solvent waste.
Important applications have been developed for the analysis of
pharmaceutical drugs, natural products, fatty acids, vitamins, pesticides,
lipids and chiral compounds. See Figure 3 on page 16.
Columns
In contrast to reversed phase separation, there is no universal stationary
phase available for SFC separations. Most typically used stationary phases are
ethyl pyridine, diol, cyano, amino, Silica and SCX columns. This usually leads
to additional effort to screen different columns in order to achieve optimum
separation. On the other hand, it provides a valuable tool for achieving
different selectivities for a given analyte mixture. A review of column
developments for SFC was recently published by T.Berger, B.Berger &
R.E.Majors in LCGC North America, May 1, 2010
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>dcZmX]Vc\Z
2
Site Requirements and Specifications
Side Requirements 18
Power Considerations 18
Power Cords 19
Bench space 20
Environment 21
Ventilation 21
Specifications 22
System Specifications 22
Specifications 22
Agilent 1260 Infinity System 26
Agilent Technologies 17
2 Site Requirements and Specifications
Side Requirements
Side Requirements
Power Considerations
The module power supply has wide ranging capability. It accepts any line
voltage in the range described in Table 6 on page 27. Consequently there is no
voltage selector in the rear of the module. There are also no externally
accessible fuses, because automatic electronic fuses are implemented in the
power supply.
The module is partially energized when switched off, as long as the power cord is
WA R N I N G
plugged in.
Repair work at the module can lead to personal injuries, e.g. electrical shock, when
the cover is opened and the module is connected to power.
Always unplug the power cable before opening the cover.
Do not connect the power cable to the instrument while the covers are removed.
Power Cords
Different power cords are offered as options with the module. The female end
of all power cords is identical. It plugs into the power-input socket at the rear
of the module. The male end of each power cord is different and designed to
match the wall socket of a particular country or region.
Bench space
G4301 Aurora SFC Fusion A5 module
The Aurora SFC Fusion A5 Module requires approximately 1 foot of linear
bench space immediately adjacent to the target Agilent 1260 Infinity system
stack. Approximately 5 inches of free space is required behind the instrument
for cable access and adequate air flow for ventilation. Similar access to the
rear of the 1260 Infinity system is also required to install cables and interface
cards. As mentioned earlier, for optimal performance, the rear air space
should not be heated significantly above room temperature by the exhaust of
other instrumentation in the lab; rather, hot exhaust should be vented or
directed upward from the instrument.
The module is designed to be installed on either side of the 1260 Infinity
system stack with sufficient high pressure transfer tubing to attach to a
double-stacked system. If the 1260 Infinity system is attached to a split-flow
detector such as Mass Spec or ELSD, the Aurora SFC Fusion A5 module
should be positioned on the opposite side of the stack. Shelves overhanging
the Aurora SFC Fusion A5 module should provide a minimum of 6 inches of
clearance to allow access to the rear power switch. Finally, the PC system
interface to the Aurora SFC Fusion A5 module is USB 2.0. A six-foot cable is
supplied with the system. The CPU must be placed within range of this cable.
Alternately, the user may supply an extended length USB cable not to exceed
16 feet.
While the Aurora SFC Fusion A5 module can exist on either side of the 1260
Infinity system, it is often easier to locate it on the left side. For more
specification details see Aurora SFC Fusion A5 on page 22
Agilent modules
The dimensions and weight of your module (see Agilent 1260 Infinity
System on page 26) allow it to be placed 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) at the rear for the circulation of air and
electric connections.
The module should be operated in a horizontal position.
Environment
Condensation within the module
CAUTION
Condensation will damage the system electronics.
Do not store, ship or use your module under conditions where temperature
fluctuations could cause condensation within the module.
If your module was shipped in cold weather, leave it in its box and allow it to warm
slowly to room temperature to avoid condensation.
Ventilation
Specifications
System Specifications
Type Specifications
Personal injury
WA R N I N G
The G4301 A Aurora SFC Fusion A5 module is heavy.
Enlist the aid of a co-worker to share the lifting load to avoid personal injury.
Type Specification
Weight 26 kg
56 lbs
Type Specification
Operating temperature 15 - 30 C
Laboratory ventilation minimum 6 air exchanges/hr for lab air; CO2 monitor
recommended w/ alarm @ 5000 ppm
Type Specifications
Inlet CO2 phase vapor from non-dip-tube high pressure cylinder; liquid
from commercial CO2 delivery system
Type Specifications
Table 3 Wetted Materials Specifications for the G4301 A Aurora SFC Fusion A5
Type Specifications
High pressure flow path 300 and 400 series stainless steel PEEK, carbon filled
PEEK PTFE, PTFE, FEP, CTFE UHMW PE ruby, sapphire,
ceramic
Low pressure flow paths [waste, wash 316 stainless steel PEEK PTFE, PTFE, FEP, CTFE CPE;
pump, leak tray] LDPE Tygon PVC
Performance Specifications
Table 4 Performance Specifications of the G4301 A Aurora SFC Fusion A5
Type Specifications
Back Pressure Regulation (BPR) system Low volume diaphragm type with proprietary drive
control; replaceable BPR head assy; No recalibration
required after head replacement
Type Specifications
Backpressure accuracy 1 %
Control and data evaluation Agilent ChemStation for LC with SFC Fusion A5 driver;
Aurora A5 Diagnostic Program
Analog in pressure monitoring 1 V FS; one input; range set by calibration to host pump
1
This temperature range represents the technical specifications for this instrument. The tempera-
tures mentioned may not be suitable for all applications and all types of solvent.
The G1322 Vacuum Degasser has been tested for evaporation of solvents into the
NOTE atmosphere by an independent institute with approved methods. The tests were performed
with Methanol (BIA Nr. 7810) and Acetonitrile (NIOSH, Nr. 1606). Evaporation of these
solvents into the atmosphere when operating the degasser was below the limits of
detection.
Safety standards: IEC, CSA, Installation category II, Pollution degree 2 For indoor use only.
UL
ASTM: Standard Practice for Testing Variable Wavelength Photometric Detectors Used in
NOTE Liquid Chromatography.
Reference conditions: cell path length 10 mm, time constant 1 s (equal to response time
2 s), flow 1 mL/min LC-grade Methanol, slit width 4 mm.
Linearity measured with caffeine at 265 mm.
Type Specification
Wavelenghth accuracy 1 nm
Data rate 80 Hz
Cell volume 13 L
Safety standards: IEC, CSA, Installation category II, Pollution degree 2 For indoor use only.
UL
Type Specification
Safety standards: IEC, CSA, Installation category II, Pollution degree 2 For indoor use only.
UL
For use with flow rates below 500 L/min, or for use without damper and mixer, a vacuum
NOTE degasser is required.
All specification measurements are done with degassed solvents.
Type Specification
Precision of flow rate Same as G1312B, ?0.07 %0.07 RSD or ?0.02 min SD,
whatever is greater based on retention time at
constant room temperature
Safety standards: IEC, CSA, Installation category II, Pollution degree 2 For indoor use only.
UL
Type Specification
3
Installing the G4309A Agilent 1260
Infinity SFC System
Hardware Installation 34
General Procedures 34
Installing G4301 A Aurora SFC Fusion A5 37
Preparing the HPLC 55
Software Installation 68
Installing Aurora SFC Fusion A5 Driver Software 68
This chapter provides an overview of the installation and setup of the hardware
and software
Agilent Technologies 33
3 Installing the G4309A Agilent 1260 Infinity SFC System
Hardware Installation
Hardware Installation
General Procedures
Proper use of wrenches
Some of the plumbing connections require a nut to be tightened onto a fitting.
There are often two sets of flats next to each other. Attempting to tighten the
nut without securing the other part of the fitting with a second wrench can
result in loosening yet another connection upstream or downstream. It is best
practice to always hold the fitting with one wrench while tightening or
loosening another connection.
Preparation
Locate all modules, devices and supporting equipment before continuing.
Ensure that the supply tubing can reach a physically secured source of CO2.
Ensure that adequate venting is available and within reach of supplied waste
systems.
This document describes a particular order of plumbing the system, with
plumbing and electrical connections described last. These operations are
performed at the rear of the systems. Depending upon your individual
installation, you may wish to perform operations at the rear of the
instruments first. This is perfectly acceptable, provided you can maintain
access to supply connections to ensure integrity and leak tightness of fittings
and connections.
Damaged Packaging
When you receive your G4301 A Aurora SFC Fusion A5 module, inspect the
shipping boxes for any signs of damage. If the shipping container or
cushioning material is damaged, notify the carrier and save the shipping
material for inspection. Save all materials until the contents have been
checked for completeness and the instrument has been mechanically and
electrically checked.
Signs of damage
CAUTION
If there are signs of damage to the G4301 A Aurora SFC Fusion A5 Module, please
do not attempt to install or use the instrument.
Delivery Checklist
Compare the delivery checklist with the contents of the shipping boxes to
ensure completeness of the shipment.
For parts identification see Parts for Maintenance on page 111. Please
report missing or damaged parts to your local Agilent Technologies
representative.
Proper system operation requires adequate space in the waste bottle to allow gaseous exit.
NOTE It is the responsibility of the operator to ensure that the waste bottle is empty before
beginning operation of the A5, and to monitor and empty the waste bottle as needed during
usage. This is not a warning.
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Locate and assemble the waste bottle and Tygon vent tubing. The vent tubing
can be placed over the spout on the top of the waste bottle. Route the Tygon
tubing to an appropriate vent. The system must be actively vented.
Locate the A5 Waste line. Insert the free end through a hole in the top of the
waste bottle cap. Insert the tube half-way into the waste bottle. Connect the
fitting end to the outlet union on the BPR. This union uses a 10-32 CPI fitting.
Tighten snugly.
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AZ[i]ZViZmX]Vc\ZgVY_jhiZYid G^\]i]ZViZmX]Vc\Zg^hjhZYid
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I]^hiZbeZgVijgZVY_jhibZci]Vh
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Figure 9 Plumbing the Agilent 1290 Infinity Thermostatted column compartment
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If the autosampler has been upgraded, the plumbing connections can be made
to the injection valve.
In the external loop operation of the autosampler, all connections are made on
the injection valve as shown. Port 1 is connected to the inlet of the right side
(column pre-heater) thermal conditioning block of the oven.
Port 6 is connected to the output flow from the binary pump.
6*jbeigVch[Zga^cZVhhZbWan
This tube can be routed through the tee slots on the side of the Aurora SFC
Fusion A5. The tube is routed upward between the Aurora SFC Fusion A5
and the Agilent 1260 Infinity stack to the bottom side of the binary pump. The
tube is then routed horizontally to the bottom center of the binary pump
where it can enter the concave opening behind the cover. The tube should then
be routed to the left side of the pump beneath the Channel A (left side). The
end of the booster transfer tube can then be installed with the adapter in the
passive inlet valve.
Any spare tubing can be located between the A5 and HPLC stack.
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The outlet of the injector wash pump is connected to the metering device in
the Agilent autosampler. To plumb the outlet side of the injector wash pump,
locate the was pump transfer line with check valve and install it in the upper
port of the injector wash pump. Flow through the wash pump is in the upward
direction. The injection wash system will not function if the check valve is
improperly installed. An arrow embossed on the check valve body indicates
the direction of flow; verify that the check valve is firmly installed.
Connect the wash pump transfer line with the spring loaded check valve. A
union is provided on the other side of the of the wash pump transfer line.
Follow instructions below for priming the injector wash pump before
connecting the union and the autosampler metering device.
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Individual cylinders
CO2 cylinders can be dangerous if handled improperly
WA R N I N G
Carbon dioxide in cylinders is partially liquefied under high pressure and contains a
great deal of energy. If containment is breached (a break in the line or cylinder) the
entire contents will vaporize and quickly expand up to 500 times in volume and
create very forceful high velocity gas streams. Cylinders must be properly
constrained, and proper tubing used, to avoid damage that could generate
projectiles.
Be sure the cylinder is properly constrained and cannot tip over. Suitable
chains or cylinder straps are required.
Cylinders in the USA and Canada use a CGA 320 cylinder adapter. One is
included in the Fusion USA ship kit, along with a 1/4 inch FNPT to 1/8 inch
compression fitting, and 6 feet of 1/8 inch OD stainless steel tubing. The filter
fitting sticking out the back of the Aurora SFC Fusion A5 module contains
1/8 inch nut and ferrule(s), which could be used with the Aurora-supplied
6 feet tube, or a longer, user-supplied tube, to connect a cylinder to the Fusion
module.
There are at least four different European standards for the connection of
carbon dioxide cylinders. They do not appear to change at national borders
(some users in one country have different supply connections from other
users in the same country). Aurora recommends that customers in Europe
contact their gas supply companies and ask them how to mate the cylinders
they supply with an American 1/8 OD supply line. This should require a
cylinder connector and a reducing union down to a 1/8 inch compression
fitting.
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Cable connections to the Aurora SFC Fusion A5 are dependent upon the
installed configuration. The primary decision to be made is whether or not an
Agilent autosampler is present. When an Agilent 1260 Infinity SFC
Autosampler is present, the Aurora SFC Fusion A5 remote line and relay
contacts lines are connected to the autosampler.
The Binary pump analog output signal should be connected to the Aurora SFC
Fusion A5 Reference in terminal.
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Lastly, a cable should be connected to the Aurora SFC Fusion A5 USB port.
This can be run to any convenient, compatible USB port on the PC.
CAN cabling between the Agilent 1260 Infinity modules is unchanged from the
normal, recommended means of interconnecting HPLC devices.
The Agilent 1260 infinity stack requires a LAN connection to the PC. This LAN
connection requires all the normal HPLC/ChemStation properties such as
BOOTP, Firewall, and IP Address settings. These remain unchanged in an
Aurora SFC Fusion A5 installation.
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Figure 19 Diagram of the Agilent Binary Pump
The G4303A SFC Pump is a binary high pressure mixing pump, optimized for
the usage in a SFC System. The Purge Valve is mounted on the right side for
purging the Modifier Channel (Channel B) only. An additional third Outlet
Ball Valve (OBV) is installed with a Valve Holder on Pumphead B, to allow the
Channel B to be flushed, even if CO2 tank pressure is supplied to the System.
The BNC coaxial cable can be used to connect the Analog Output on the back
panel of the Binary pump to the SFC Fusion A5 Reference In
terminal/connector on the back of the Fusion module. Be aware that the
output of similar appearance on the DAD and VWD detectors should NOT be
used.
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Replacing a rotor seal is well documented in Agilent manuals, and service videos. Please
NOTE refer to these guides for further assistance.
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Figure 22 Autosampler Fluidic connections
2 Connect one end of the wash pump transfer line with the check valve to the
outlet port of the injection wash pump.
3 Before connecting the union end of the wash pump transfer line, use a
syringe and Luer Adapter to prime (pull sample through) the injection wash
pump
4 The existing line (blue capillary) from the inlet of the Agilent 1260 Infinity
SFC Autosampler metering device can be plumbed into the union on the
wash pump transfer line
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Take the BCD Interface card from the shipping kit, taking care to prevent
damage from static electricity, solvent, etc.
Electronic boards are sensitive to electrostatic discharge (ESD) and should be handled
CAUTION
with care so as not to damage them. Touching electronic boards and components can
cause electrostatic discharge.
ESD can damage electronic boards and components.
Be sure to hold the board by the edges and do not touch the electrical components.
Always use an ESD protection (for example, an ESD wrist strap) when handling
electronic boards and components.
1 Carefully slide the board into the slot. When it is fully in place, gently push
the bezel until the connectors engage. Tighten the captive knurled nuts.
2 With the BCD card in place, connect the 15-pin relay contacts connector to
the relay input connector on the back of the Aurora SFC Fusion A5.
3 Connect the 9-pin Remote connector on the back left of the autosampler to
the 9-pin Remote connector on the back of the Aurora SFC Fusion A5.
Injection
Time
Stoptime No Limit
Posttime Off
High Throughput
Needle Wash
Repeat 1 times
Injector Cleaning
Valve Movements 1
Auxiliary
Store Temperature No
Row Action
1 NEEDLE down
2 CONTACT B CLOSED
4 CONTACT B OPEN
5 VALVE bypass
12 CONTACT B CLOSED
14 CONTACT B OPEN
Contact 1 Open
Contact 2 Open
Contact 3 Open
Contact 4 Open
Using the Agilent SFC Autosampler as a fixed loop to (external) loop autosampler has
NOTE several minor consequences that need to be understood to achieve adequate performance.
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If a large loop is used, air bubbles can be used to displace the wash solvent.
Software Installation
3 Confirm installation.
4
Configuring the System
Configuring SFC interface in ChemStation 72
Setting up the Method 76
Status 78
Control 79
Testing the System 80
How to configure the Agilent 1260 Infinity SFC Analytical system and G4301 A
Aurora SFC Fusion A5 in ChemStation with Aurora add-on drivers.
Agilent Technologies 71
4 Configuring the System
Configuring SFC interface in ChemStation
The Aurora SFC Fusion A5 ChemStation interface works with the ChemStation Modular
NOTE LC System, not with Modular LC System (Classic). The Modular LC System (Classic)
instrument does not support RC.Net drivers, which are necessary for the LC modules.
6 To set up the SFC module, scroll down the Configurable Modules slider until
you see the SFC icon. Select it with a double-click or right arrow to move it
to the Selected Modules panel.
8 In the Aurora SFC Configuration, enter the device name or use the default to
identify the module within Agilent ChemStation. Select a COM Port in the
Aurora COM Port field.
1 In the Agilent ChemStation, the method parameters for all RC.Net devices,
including SFC settings, are combined into a single tabbed dialog box:
2 The Instrument Curves tab shows all instrument curves (monitor traces)
available for storing with the acquired data file:
Status
Control
The following steps show you how you can control your SFC instrument in the
Agilent ChemStation.
1 In Instrument > More SFC you find more menu items that allow you to control
the Aurora device directly.
The SFC driver lists all available configuration, method and status values in
ChemStation registers, available by macros.
5
Using the Aurora SFC Fusion A5
Powering up the Module 82
Power-up Sequence and Operational Control States 83
Operational Control States 84
Controlling the Aurora SFC Fusion A5 through the Agilent
ChemStation 87
Running a method on the SFC system 89
Shutting Down the SFC System 92
Partial Shutdown 92
This chapter provides information and hints on the use of the SFC System.
Agilent Technologies 81
5 Using the Aurora SFC Fusion A5
Powering up the Module
The Aurora SFC Fusion A5 module is powered on by pressing the top of the
rocker-type power switch located on the upper right rear of the module. Once
the rocker is pressed, the Aurora SFC Fusion A5 module responds by
entering its power-up sequence. The power button of the Aurora SFC Fusion
A5 unit must remain accessible at all times. Never arrange equipment so that
the switch cannot be accessed.
The Aurora SFC Fusion A5 module has three defined operational control
states: OFF, STANDBY and ON. You control the three states by selecting the A5
Control option from either the ChemStation SFC Fusion icon, by pressing
various icons of the ChemStation GUI, or from the Aurora A5 Diagnostic
Program status tab.
Some components of the Aurora SFC Fusion A5 module are not governed by
the three described states but are continuously on. These include:
The processor.
Continuously records and transmits sensor data to the host control
system.
Handles status and command requests from the host controller.
Monitors sensors for safety-related parameters.
Updates the event log.
Pressure and temperature sensors are continuously powered and sensed.
Coolant and electronics bay fans are continuously powered.
The wash pump is activated by contact closure of the external contacted
board placed in the SFC Autosampler, independent of the Aurora SFC
Fusion A5 control state.
When the Aurora SFC Fusion A5 Module is in the STANDBY state, the two
status lights flash alternately. The STANDBY state remains active for up to
three hours. If no user-initiated action is taken to change or renew the state
within this time, a timeout occurs and the processor automatically enters the
OFF state.
The ON State
The ON state is characterized as follows:
The CO2 supply valve is open (powered).
The booster pump drive is powered and begins to pump CO2 to the pressure
target.
The BRP drive is powered and the BRP begins the process of regulating to
its setpoint.
The BRP heater is powered.
The chiller is powered.
The secondary cooling circuit pump is powered.
The ON state can also be entered by selecting the On option in the control
window, by pressing the power button associated with the SFC icon of the
GUI, or by pressing On in the ChemStation graphical user interface.
When the Aurora SFC Fusion A5 Module is in the ON state, the top status
light is continuously lit. The bottom status light is lit when the system reaches
a ready state, indicating that backpressure and booster pump pressure are
under control and stabilized within their control band.
Modules that start from the OFF state generally must first perform an
initialization routine before moving to ON. In the case of the Aurora SFC
Fusion A5 module, initialization causes the BPR first to home, then move to
a default initialization position. The booster pump delays operation until the
chiller passes below a threshold temperature value.
Editable method parameters for the Aurora SFC Fusion A5 are the Nozzle
Pressure (system back-pressure) and the Nozzle Temperature (temperature of
the back-pressure regulator).
When the wash pump icon is clicked, the wash pump starts pumping for 30
seconds and flushes the autosampler metering, loop, needle and needle seat
with solvent, Typically, modifier solvent is used to flush the autosampler. The
wash pump is controlled by the Agilent SFC autosampler via the built-in BCD
board, and works independently of the current state of the Aurora Fusion A5.
The manner of shutting down the SFC depends on the requirement for rapid
equilibration of the system on the next startup, and the duration of the
shutdown. If the system will be shut down for some time, it is probably best to
shut down all components including the DAD and column oven. These
components tend to take longer to reach their stable operating conditions than
the other components in the system. You should always shut down both the
Aurora SFC Fusion A5 and the binary pump if the system is to be idle for a
long time.
Partial Shutdown
Injuries from pressurized CO2
WA R N I N G
Setting the pump to STANDBY does not depressurize the system. Do not attempt to
loosen fittings or perform maintenance under these conditions. Serious skin and
eye injuries can occur as the result of sudden release of CO2 in the liquid or
supercritical state. Always wear gloves and eye protection when maintaining the
Aurora SFC Fusion A5 unit.
two hours elapse in STANDBY mode, the Aurora SFC Fusion A5 enters the
OFF state, and pressure may be lost at a more rapid rate.
If the Aurora SFC Fusion A5 unit itself is to be serviced, select OFF in the Control window.
NOTE This shuts off the BPR heater and booster chiller and allows them to move toward ambient
temperature.
This causes the BPR to home and fully open the CO2 path to depressurize. The
Aurora SFC Fusion A5 unit contains approximately 25 mL of stored CO2.
This amount of CO2 should be vented properly, which takes several minutes.
You should allow the system to drain below 40 bar before cracking any fittings.
At this point the, CO2 is in the vapor state, and represents a small expanded
volume. However, do not inhale vapor directly from a cracked fitting. The
concentration of CO2 emerging from a flow line, even at low pressure, can be
dangerous or even lethal.
Alternatively, if the column oven contains a column switching valve, one path
may be jumpered without a column. The reduced restriction will allow the
system to depressurize much faster. Further, the isolated column can be
exchanged immediately since the contained volume of CO2 is small.
6
Maintenance and Repair
Inspection and Preventative Maintenance Intervals 96
Daily Inspection and Maintenance 96
Every 3 months 97
Annually 97
As Needed (Corrective) 98
General Maintenance procedures 99
Booster Drawer 99
Replacing Fuses 107
Standard Decontamination 108
Plugged BPR Decontamination 109
Preparing for storage or shipping 109
In this chapter only the SFC specific procedures are described. For procedures
similar to the Agilent module procedures, please refer to the single module
manuals (G1312C, G1329B, G1316C, G1315/65C, G1322A)
Agilent Technologies 95
6 Maintenance and Repair
Inspection and Preventative Maintenance Intervals
Inspection and maintenance are critical elements of long term reliability and
performance of the Agilent 1260 Infinity Analytical SFC System. Maintenance
falls into two categories: preventative and corrective. Preventative
maintenance intervals vary based on system use. The intervals offered in this
section are for systems with average use of approximately 30 hours per week.
The preventive maintenance intervals can be extended for infrequently used
systems, while heavily used systems may require more frequent preventative
maintenance. Most service can be performed directly by the user or by
in-house maintenance technicians.
Every 3 months
Run nozzle diagnostic test.
Run system leak test.
Evaluate system calibration.
Check chiller efficiency curve.
If CO2 cylinders are used as supply, change the cylinder seal (approximately
every 10 cylinders) at the next tank change.
Remove visible dust accumulation in the area of the module.
Annually
Have service evaluation and maintenance by a qualified Agilent service
technician.
Perform 3-month maintenance.
Change coolant.
Clean fan access paths.
Upgrade firmware with any recommended safety or performance
enhancements.
Change wash line check valve.
Change injection valve 3-groove rotor.
Inspect high pressure flow cell.
Inspect leak sensor function.
Change pump seals SFC Pump.
Change purge valve frit.
Change needle and needle seat in the autosampler.
Change boaster pump seal.
As Needed (Corrective)
Change booster and CO2 pump check valves.
Change high pressure transfer lines with metal ferrules or PEEK end
fittings after 10-20 reseals or when leaking.
Change Booster piston (rare).
Exchange BPR head (rare).
Booster Drawer
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Tools required A 3/16 hex-drive wrench (mounted on the back of the front cover)
1 Set the Control state to OFF on the Aurora SFC Fusion A5 module.
2 Wait for the chiller temperature to approach room temperature to prevent
significant condensation on the chiller assembly and pump head.
3 Turn the power OFF on the Aurora SFC Fusion A5 module. Unplug the
power cord.
4 Remove the front cover of the Aurora SFC Fusion A5 unit by pulling
gently at the upper left and right indents to the rear of the cover. The cover
will release from its magnetic catch. Lift the cover upward to clear the two
mounting pins at the base and set it aside.
The 3/16 hex wrench used to remove the vapor shield and pump head is stored inside the
HINT removable front cover.
5 While holding the vapor shield with one hand, use the 3/16 hex wrench to
loosen the four cap screws attaching each corner of the shield until they
each disengage from the front panel. The screws are captured in the shield;
do not try to remove them completely.
6 Remove the shield and store it in a safe location. Do not use a container for
disassembled parts. This will scratch the plastic and impair visibility of the
pump head during operation.
6 Insert the new check valve cartridge into the holder oriented correctly for
the direction of flow (arrow up). The inlet check valve is inserted with the
non-filter end of the cartridge showing. The outlet check valve is inserted
with the filter end of the cartridge showing.
7 Replace the PEEK gasket on the top of the inlet check valve cartridge with
the flat side of the gasket facing the cartridge. (Inlet CV only)
8 Insert the CV holder into the pump head and tighten with a 9/16 wrench.
9 Refasten the inlet or outlet capillary line, holding the CV holder with a
9/16 wrench, and tightening the fitting with the 1/4 wrench to seal.
10 Replace the vapor shield
Each time the booster pump head is removed, the piston seal should be exchanged, since
NOTE the seal surface may be easily scratched or distorted during removal. For this reason, the
procedures are bundled. Cleaning the pump head is optional after visual inspection. Sealing
surfaces of the pump head are critical to successful operation. Never use metal tools or
paper toweling to wipe, probe or contact these surfaces.
5 Using the 9/16 and 1/4 wrenches, remove the inlet line from the inlet
check valve holder and the outlet line from the outlet check valve holder.
Danger of piston breakage
CAUTION
Be careful not to break the piston when removing the pump head. Twisting the
pump head can cause the piston to break.
6 Using the 3/16 hex-drive, carefully remove the two knurled nuts at the
front of the pump head.
7 Carefully separate the pump head from the pump. Move the pump head
straight out from the pump and remove it from the piston. Be careful not to
break or damage the piston. Also remove the seal from the piston if it did
not stay in the pump head.
8 If the seal remains with the pump head, insert the flanged end of the seal
insertion/removal tool into the seal cavity. Tilt it slightly so that flange is
under the seal and pull out the seal.
Tools required Tools for removing the vapor shield (see Removing the vapor shield on page 100) and pump
head (see Removing the Pump head on page 102)
A 9/64 hex-drive wrench
In most cases, this procedure will be used only to replace a broken piston. Pumping CO2
NOTE
does not tend to leave deposits on the piston. Development of such deposits warrants
examination of the CO2 supply system and correcting the source of the deposited materials.
Release of extraneous materials into the CO2 supply system may cause contamination of
the Agilent 1260 Infinity Analytical SFC System.
4 With a gentle rocking motion, loosen the chiller plate assembly and
carefully slide it forward off the pump head mounting posts. Carefully twist
the assembly out of the way.
5 Use the 9/64 hex wrench to unscrew the two cap screws attaching the
spacer and very carefully remove the spacer by pulling straight back. This
fully exposes the piston and retaining ring.
6 Remove the retaining ring by prying it out with a small blunt instrument or
tweezers at the slot provided.
7 Grasp the metal base of the piston assembly so that you avoid exerting any
side load on the sapphire rod, and remove the piston from the slot in the
carrier by sliding it up.
8 Grasp the metal base of the replacement piston assembly, and insert it into
the slot in the piston carrier until it bottoms in the slot.
9 Replace the retaining ring and spacer. Reattach the spacer mounting
screws. If properly positioned, the spacer should be pressed into the foam
wall seal.
10 Gently slide the chiller back onto the pump mounting posts and firmly
press it onto the spacer. If properly positioned, the chiller heat exchanger
should now be pressed into the foam wall seal.
11 Replace the piston seal
12 Replace the pump head
13 Replace the vapor shield
Replacing Fuses
The power entry module of the Aurora SFC Fusion A5 unit contains an
external fuse drawer that is user serviceable.
To replace fuses: (before replacing fuses, first try to determine cause of fuse
activation and repair)
Standard Decontamination
Cleaning
External surfaces of the enclosure can be wiped with a damp soft cloth. More
stubborn marks can be removed with a 50 % isopropanol:water mixture or
mild cleanser such as Soft Scrub. The latter may also be used to remove
surface paint blemishes that may result from normal use.
The vapor shield of the booster drawer should be wiped only with a very soft
cloth such as a microfiber polypropylene cloth, otherwise the surface may be
scratched. Other user-accessible internal surfaces can be cleaned with a damp
cloth.
BPR
The BPR head contacts CO2, modifiers and sample material. To
decontaminate, rinse with 50 % modifier flow at 5 mL/min for 15 min followed
by pure CO2 for 5 min.
Wash Pump
1 Drain the inlet line of old solvent.
2 Flush the inlet line and filter from a small intermediate reservoir to rinse
contaminated residual fluid from the lines.
3 Insert the inlet line into a fresh supply of pure solvent
4 Prime the wash pump for 2 min (four consecutive presses of the 30 s timer)
to clear the remaining flow path.
8 Disconnect the booster pump transfer line from the binary pump at the
pump inlet check valve.
9 Disconnect the BPR return line from the detector.
10 Coil both lines to fit inside the A5 unit behind the removable front panel.
11 Replace the front panel
12 Disconnect the power cord and all signal cables from both ends of the
connection.
13 Store cables and cords in a large plastic zip-lock bag.
14 Cover the unit with a large plastic bag.
15 If the original container is available, place the unit with its left side down in
the packaging. Otherwise, store the unit upright in the storage area.
16 If the HPLC will also be stored or shipped, and will be reconfigured as an
SFC system, the upgrade components can remain in the system.
17 If the two systems are to be permanently separated, uninstall the check
valves, modifier purge valve, 3-groove rotor and high pressure flow cell by
reversing the installation procedures in Hardware Installation on page 34.
Store the components along with the original software disc and any
upgrades with the module.
7
Parts for Maintenance
G4301 A Aurora SFC Fusion A5 Parts 112
Agilent Module Parts 114
p/n Description
G4301-65000 Mainboard
G4301-60500 Nozzle
&%
.
&
)
+
-
'
*
Figure 31 Agilent 1260 Infinity SFC Binary Pump specific SFC Parts
p/n Description
G1312-87330 Mixer
For all other Part Numbers please refer to the G1312B User manual.
NOTE
p/n Description
For all other Part Numbers please refer to the G1329B User manual.
NOTE
p/n Description
For all other Part Numbers please refer to the G1315/65C User manual.
NOTE
8
Identifying Cables
A5 Cables 120
Overview 121
BCD Cables 123
External Contact Cable 125
CAN/LAN Cables 126
Auxiliary Cable 127
RS-232 Cables 128
This chapter provides information on cables used with the Agilent 1200 Infinity
Series modules.
A5 Cables
p/n Description
Overview
Never use cables other than the ones supplied by Agilent Technologies to ensure proper
NOTE functionality and compliance with safety or EMC regulations.
BCD cables
p/n Description
Auxiliary
p/n Description
CAN cables
p/n Description
RS-232 cables
p/n Description
LAN cable
p/n Description
5023-0202 Twisted pair network cable, shielded, 7 m (for point to point connection)
BCD Cables
p/n G1351-81600 Wire Color Pin Agilent Signal Name BCD Digit
module
Green 1 BCD 5 20
Violet 2 BCD 7 80
Blue 3 BCD 6 40
Yellow 4 BCD 4 10
Black 5 BCD 0 1
Orange 6 BCD 3 8
Red 7 BCD 2 4
Brown 8 BCD 1 2
not connected 14
p/n 03396-60560 Pin 3396 Pin Agilent Signal Name BCD Digit
module
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
5 1
10 6
15 11
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
CAN/LAN Cables
p/n Description
LAN Cables
p/n Description
5023-0202 Twisted pair network cable, shielded, 7 m (for point to point connection)
Auxiliary Cable
White 1 Ground
Green 3
Yellow 4
Grey 5 DC + 5 V IN
Pink 6 Vent
RS-232 Cables
p/n Description
9
Appendix
General Safety Information 130
The Waste Electrical and Electronic Equipment (WEEE) Directive
(2002/96/EC) 133
Radio Interference 134
Sound Emission 135
Solvent Information 136
Agilent Technologies on Internet 137
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 customers failure to comply with
these requirements.
Safety Standards
This is a Safety Class I instrument (provided with terminal for protective
earthing) and has been manufactured and tested according to international
safety standards.
Operation
Before applying power, comply with the installation section. Additionally the
following must be observed.
Do not remove instrument covers when operating. Before the instrument is
switched on, all protective earth terminals, extension cords,
auto-transformers, and devices connected to it must be connected to a
protective earth via a ground socket. Any interruption of the protective earth
grounding will cause a potential shock hazard that could result in serious
personal injury. Whenever it is likely that the protection has been impaired,
the instrument must be made inoperative and be secured against any intended
operation.
Make sure that only fuses with the required rated current and of the specified
type (normal blow, time delay, and so on) are used for replacement. The use of
repaired fuses and the short-circuiting of fuse holders must be avoided.
Some adjustments described in the manual, are made with power supplied to
the instrument, and protective covers removed. Energy available at many
points may, if contacted, result in personal injury.
Any adjustment, maintenance, and repair of the opened instrument under
voltage should be avoided whenever possible. When inevitable, this has to be
carried out by a skilled person who is aware of the hazard involved. Do not
attempt internal service or adjustment unless another person, capable of
rendering first aid and resuscitation, is present. Do not replace components
with power cable connected.
Do not operate the instrument in the presence of flammable gases or fumes.
Operation of any electrical instrument in such an environment constitutes a
definite safety hazard.
Do not install substitute parts or make any unauthorized modification to the
instrument.
Capacitors inside the instrument may still be charged, even though the
instrument has been disconnected from its source of supply. Dangerous
voltages, capable of causing serious personal injury, are present in this
instrument. Use extreme caution when handling, testing and adjusting.
When working with solvents please observe appropriate safety procedures
(e.g. goggles, safety gloves and protective clothing) as described in the material
handling and safety data sheet by the solvent vendor, especially when toxic or
hazardous solvents are used.
Safety Symbols
Table 15 Safety Symbols
Symbol Description
The apparatus is marked with this symbol when the user should refer to the
instruction manual in order to protect risk of harm to the operator and to
protect the apparatus against damage.
Indicates eye damage may result from directly viewing the light produced
by the deuterium lamp used in this product.
The apparatus is marked with this symbol when hot surfaces are available
and the user should not touch it when heated up.
A WARNING
WA R N I N G
alerts you to situations that could cause physical injury or death.
Do not proceed beyond a warning until you have fully understood and met the
indicated conditions.
A CAUTION
CAUTION
alerts you to situations that could cause loss of data, or damage of equipment.
Do not proceed beyond a caution until you have fully understood and met the
indicated conditions.
Abstract
The Waste Electrical and Electronic Equipment (WEEE) Directive
(2002/96/EC), adopted by EU Commission on 13 February 2003, is
introducing producer responsibility on all Electric and Electronic appliances
from 13 August 2005.
NOTE
This product complies with the WEEE Directive (2002/96/EC) marking requirements. The
affixed label indicates that you must not discard this electrical/electronic product in
domestic household waste.
Product Category: With reference to the equipment types in the WEEE Directive Annex I,
this product is classed as a Monitoring and Control instrumentation product.
Do not dispose off in domestic household waste
To return unwanted products, contact your local Agilent office, or see www.agilent.com for
more information.
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
Manufacturers 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
Flow Cell
To protect optimal functionality of your flow-cell:
Avoid the use of alkaline solutions (pH > 9.5) which can attack quartz and
thus impair the optical properties of the flow cell.
Use of Solvents
Observe the following recommendations on the use of solvents.
Brown glass ware can avoid growth of algae.
Avoid the use of the following steel-corrosive solvents:
Solutions of alkali halides and their respective acids (for example,
lithium iodide, potassium chloride, and so on),
High concentrations of inorganic acids like sulfuric acid and nitric acid,
especially at higher temperatures (if your chromatography method
allows, replace by phosphoric acid or phosphate buffer which are less
corrosive against stainless steel),
Halogenated solvents or mixtures which form radicals and/or acids, for
example:
2CHCl3 + O2 2COCl2 + 2HCl
This reaction, in which stainless steel probably acts as a catalyst, occurs
quickly with dried chloroform if the drying process removes the
stabilizing alcohol,
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.
For the latest information on products and services visit our worldwide web
site on the Internet at:
http://www.agilent.com
Select Products/Chemical Analysis
It will provide also the latest firmware of the modules for download.
Index
A external contact P
cable 125
Agilent physical specifications 27, 29, 30, 31
on internet 137 power consideration 18
algae 136
F
power consumption 26, 26, 27, 29,
ambient non-operating temperature 26, flow cell 136 30, 31
27, 29, 30, 31 solvent information 136 power cords 19
ambient operating temperature 26, 27, frequency range 26, 27, 29, 30, 31
29, 30, 31 R
auxiliary H RS-232C
cable 121, 127 humidity 26, 27, 29, 30, 31 cable 128
RS-232
B I cable 121
BCD installation
cable 121, 123 power cords 19 S
site requirements 18 safety class I 130
C internet 137 safety
cable general information 130
Auxiliary 121, 127 L standards 30, 31, 27, 29
BCD 121, 123 laboratory bench 20 symbols 132
CAN 126 site requirements 18
LAN
external contact 125 solvents 136
cable 122, 126
LAN 122, 126
line frequency 26, 27, 29, 30, 31 specification
RS-232 121, 128
line voltage 26, 27, 29, 30, 31 physical 27, 26, 31, 29, 30
cables
Specifications 22
overview 121
CAN
N
non-operating altitude 26, 27, 29, 30,
V
cable 126
condensation 21 31 vacuum degasser 30
non-operating temperature 27, 29, 30, voltage range 26, 27, 29, 30, 31
31
D
W
dimensions 26, 26, 27, 29, 30, 31 O weight 26, 26, 27, 29, 30, 31
operating Altitude 26, 27, 29, 30, 31
E
operating temperature 27, 29, 30, 31
electrostatic discharge (ESD) 61
In This Book
*G4301-90100*
*G4301-90100*
G4301-90100
Rev. C
Agilent Technologies