G1312-90010 BinaryPumpSL User Ebook
G1312-90010 BinaryPumpSL User Ebook
G1312-90010 BinaryPumpSL User Ebook
User Manual
Notices
Agilent Technologies, Inc. 2006 No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws.
Warranty
The material contained in this document is provided as is, and is subject to being changed, without notice, in future editions. Further, to the maximum extent permitted by applicable law, Agilent disclaims all warranties, either express or implied, with regard to this manual and any information contained herein, including but not limited to the implied warranties of merchantability and fitness for a particular purpose. Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing, use, or performance of this document or of any information contained herein. Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate agreement shall control.
rights not conveyed under these terms, they must negotiate with Agilent to establish acceptable terms in a written agreement executed by all relevant parties.
Safety Notices
CAUTION
A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met.
Edition
02/06 Printed in Germany Agilent Technologies Hewlett-Packard-Strasse 8 76337 Waldbronn, Germany
Software Revision
This guide is valid for B.02.xx revisions of the Agilent ChemStation software, where xx refers to minor revisions of the software that do not affect the technical accuracy of this guide.
Technology Licenses
The hardware and/or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license.
WA R N I N G
A WARNING notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in personal injury or death. Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met.
In This Guide
1 Introduction to the Binary Pump SL
This chapter provides an overview of the functionality of the Binary Pump SL.
Optimizing Performance
This chapter gives information on how to optimize the performance of the Binary Pump SL under special operational conditions.
Appendix
Contents
1 Introduction to the Binary Pump SL Introduction to the Binary Pump SL Instrument Layout 12 Principle of Operation 13 Optimization Features 15 Electrical Connections Firmware Updates 2 20 18 12
Physical Specifications
30 32
Optimizing the Stack Configuration Single Stack Setup 33 Twin Stack Setup 35 Installing the Binary Pump SL 37
Flow Connections with Solvent Selection Valve Flow Connections without Solvent Selection Valve Priming the System 47 Initial Priming 47 Regular Priming 48
41 44
49
52
Setting the Pump up with the G4208A Instant Pilot Setting the Pump up with Agilent ChemStation Overview 56 Setup of Basic Pump Parameters 58 Pump Control 60 Auxiliary Pump Parameters 61 Data Curves 63 Bottle Filling 64 Early Maintenance Feedback (EMF) EMF Counters 66 Using the EMF Counters 67 5 Optimizing Performance Prevent Blocking of Solvent Filters 70 Checking the Solvent Filters 70 Cleaning the Solvent Filters 71 When to Use a Vacuum Degasser 72 Operational Hints for the Vacuum Degasser When to Use the Active Seal Wash Option When to Use Alternative Seals 74 73 72 66 56
55
When to Remove Damper and Mixer 75 Convert the Binary Pump SL to Low Delay Volume Mode How to Optimize the Compressibility Compensation Setting Solvent Compressibility Calibration 78
76 78
Optimization of Legacy Compressibility Settings 6 Tests and Calibration Functions Pressure Test 82 Running the Pressure Test 84 Evaluating the Results 85 Pump Test 87 Running the Pump Test Evaluating the Results 88 88
79
Solvent Compressibility Calibration 89 Running the Solvent Compressibility Calibration Pump Elasticity Calibration 91 Running the Pump Elasticity Calibration 7 Maintenance and Repair Introduction to Maintenance and Repair 94 Simple Repairs - Maintenance 94 Exchanging Internal Parts - Repair 94 Warnings and Cautions 95 96 92
90
Cleaning the Binary Pump SL Using the ESD Strap 8 Maintenance and Simple Repairs 97
100 102
Maintenance Procedures 101 Exchanging the Purge Valve Frit or the Purge Valve Removing the Pump Head Assembly 104 Disassembling the pump head 106 Exchanging the Pump Seals 107 Seal Wear-in Procedure 109
Exchanging the Plungers 110 Exchanging the Wash Seals 111 Reinstalling the Pump Head Assembly
113
Simple Repair Procedures 115 Exchanging the Active Inlet Valve Cartridge 116 Exchanging the Active Inlet Valve Body 118 Exchanging the Outlet Ball Valve 121 Exchanging the Solvent Selection Valve 124 Installing the Active Seal Wash Option 126 Exchanging the Optional Interface Board Replacing the Pumps Firmware 9 Parts and Materials for Maintenance Bottle Head Assembly 136 138 140 133 131
Hydraulic Path with Solvent Selection Valve Hydraulic Path without Solvent Selection Valve Pump-Head Assembly SL Outlet Ball Valve Assembly Purge Valve Assembly 145 146 142 144
148 149
Active Seal Wash Option G1312-68721 G1316B SL Capillary System Kit Optional Interface Boards A Appendix General Safety Information 154 152 150
Lithium Batteries Information Radio Interference Sound Emission 158 159 160
157
Solvent Information
162
10
This chapter provides an overview of the functionality of the Binary Pump SL.
Agilent Technologies
11
The Binary Pump SL comprises two identical pumps integrated into one housing. Binary gradients are created by high-pressure mixing. An optional degasser is available for applications that require best flow stability, especially at low flow rates, for maximum detector sensitivity. Pulse damper and mixer can be bypassed for low flowrate applications or whenever a minimal transient volume is desirable. Typical applications are high throughput methods with fast gradients on high resolution 2.1 mm columns. The pump is capable of delivering flow in the range of 0.1 - 5 mL/min against up to 600 bar. A solvent selection valve (optional) allows to form binary mixtures (isocratic or gradient) from one of two solvents per channel. Active seal wash (optional) is available for use with concentrated buffer solutions.
Instrument Layout
The industrial design of the module incorporates several innovative features. It uses Agilents E-PAC concept for the packaging of electronics and mechanical assemblies. This concept is based upon the use of expanded polypropylene (EPP) foam plastic spacers in which the mechanical and electronic boards components of the module are placed. This pack is then housed in a metal inner cabinet which is enclosed by a plastic external cabinet. The advantages of this packaging technology are: virtual elimination of fixing screws, bolts or ties, reducing the number of components and increasing the speed of assembly/disassembly, the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations, the plastic layers help cushion the electronic and mechanical parts from physical shock, and the metal inner cabinet shields the internal electronics from electromagnetic interference and also helps to reduce or eliminate radio frequency emissions from the instrument itself.
12
Principle of Operation
The Binary Pump SL is based on a two-channel, dual-piston in-series design which comprises all essential functions that a solvent delivery system has to fulfill. Metering of solvent and delivery to the high-pressure side are performed by two pump assemblies which can generate pressure up to 600 bar. Each channel comprises a pump assembly including pump drive, pump head, active inlet valve with replaceable cartridge and outlet valve. The two channels are fed into a low-volume mixing chamber which is connected via a restriction capillary coil to a damping unit and a mixer. A pressure sensor monitors the pump pressure. A purge valve with integrated PTFE frit is fitted to the pump outlet for convenient priming of the pumping system.
Mixer
Damper
to waste
Pressure sensor Outlet valve Outlet valve Inlet valve Seals Pistons Pump head B from solvent bottle B
Mixing Chamber
Figure 1
The Hydraulic Path of the Binary Pump SL with Damper and Mixer Damper and mixer can be bypassed for lowest delay volume of the Binary Pump SL. This configuration is recommended for low flow rate applications with steep gradients, see the Rapid Resolution System Manual.
13
Figure Figure 2 on page 14 illustrates the flow path in low delay volume mode. For instructions on how to change between the two configurations, see Convert the Binary Pump SL to Low Delay Volume Mode on page 76.
NOTE
Bypassing the mixer while the damper remains in line is not a supported configuration and may lead to undesired behavior of the Binary Pump SL.
Mixer Purge valve Pump outlet Pressure sensor to waste Outlet valve Inlet valve from solvent bottle A Seals
Damper
Outlet valve Inlet valve Seals Pistons Pump head B from solvent bottle B
Mixing chamber
Figure 2
The Hydraulic Path of the Binary Pump SL with bypassed Damper and Mixer Table 1 Binary Pump SL Details
From mixing point to pump outlet, dependent on back pressure 120 L without damper and mixer 600 800 L with damper and mixer
Delay volume
14
Table 1
Pump head
Active Inlet Valve Outlet Valve Adapter Purge Valve Damping Unit
Optimization Features
What is Pump Elasticity Compensation?
The flow path of the pump consists of pump chambers, sapphire pistons, polymer seals, stainless steel tubing of different dimension, pressure sensor, and so forth. All of these parts deform when pressurized. The sum of this deformation is called pump elasticity. The performance of the pump is greatly enhanced by correcting for this elasticity. The Pump Elasticity Calibration calculates correction factors to compensate for the individual elasticity of the pump that was calibrated. The elasticity is different for every pump and may change with the replacement of parts in the flow path, e.g. pump seals. All Binary Pumps SL are elasticity calibrated at the factory and require recalibration only after preventive maintenance or major repairs to the flow path. Replacement of capillaries or PTFE frits are not considered a major repair.
15
600 bar. In addition, the compressibility changes with pressure, temperature and the amount of dissolved gas. In order to minimize the influence of the latter, the use of a vacuum degasser is mandatory for high precision delivery of liquids. Unfortunately, the influence of the temperature on compressibility is non-linear and cannot be calculated. The Agilent Binary Pump SL features a new multi point compressibility calibration. The compressibility of a solvent is determined at different pressures from 0 - 600 bar and stored in an XML file. This file can be distributed to other pumps because the solvent compressibility is independent from the pump. The Binary Pump SL and ChemStation come with predetermined solvent compressibility data for the most common HPLC solvents like water, acetonitrile, methanol, etc. Users can calibrate their own solvent mixtures with the help of an easy to use calibration procedure in the Agilent LC Diagnostic software.
CAUTION
A correct pump elasticity calibration is an essential prerequisite for successful solvent compressibility calibrations! Solvent compressibility calibrations acquired with a miscalibrated pump will work, but they are not transferable to other pumps!
16
The Binary Pump SL uses a processor-controlled ball screw system to drive its pistons. The normal stroke volume is optimized for the selected flow rate. Small flow rates use a small stroke volume while higher flow rates use a higher stroke volume. The stroke volume for the pump is by default set to AUTO mode. This means that the stroke is optimized for the flow rate in use. A change to larger stroke volumes is possible but not recommended.
17
Electrical Connections
The CAN bus is a serial bus with high-speed data transfer. The two connectors for the CAN bus are used for internal Agilent 1200 Series module data transfer and synchronization. One analog output provides a pressure signal for integrators or data handling systems. The REMOTE connector may be used in combination with other non 1100/1200 Series equipment if you want to use features such as common shut down, prepare, and so on. The RS-232 connector may be used to control the Binary Pump SL from a computer via RS-232 connection, using appropriate software. This connector needs to be activated by the configuration switch module at the rear of the pump. The software needs the appropriate drivers to support this communication. See your software documentation for further information. The power input socket accepts a line voltage of 100 120 or 220 240 volts AC 10 % with a line frequency of 50 or 60 Hz. Maximum power consumption is 220 VA (Volt-Amps). There is no voltage selector on your Binary Pump SL because the power supply has wide-ranging capability. There are no externally accessible fuses, because automatic electronic fuses are implemented in the power supply. The security lever at the power input socket prevents that the Binary Pump SL cover is taken off when line power is still connected. The interface board slot is used for external contacts, BCD output or the installation of a G1369A LAN interface.
WA R N I N G
Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
18
Configuration switch Slot for interface board RS232 Remote Analog output CAN-Bus
Figure 3
WA R N I N G
To disconnect the binary pump from line, unplug the power cord. The power supply still uses some power, even if the power switch on the front panel is turned off.
Interfaces
The Binary Pump SL provides the following interfaces: two CAN connectors as interface to other Agilent 1200 Series modules, one RS-232C as interface to a computer, one REMOTE connector as interface to other Agilent products, one analog output for pressure signal output, and one slot for optional interface boards
19
Firmware Updates
Firmware updates can be done using your user interface: G4208A Instant Pilot with files from a USB-stick Agilent ChemStation with files from CD-ROM The file naming conventions are: 1312B_A601_12.dlb, or more general: xxxxx_yyyy_zz.dlb, where xxxx yyyy zz is the product number, e.g. 1316 for the G1316A TCC, and is the revision number, for example A601 is revision A.06.01, and is the build number
NOTE
Update of main system can be done in the resident system only. Update of the resident system can be done in the main system only.
resident FW update
Figure 4
20
This chapter provides information about site requirements and specifications for the Binary Pump SL.
Agilent Technologies
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Site Requirements
Power Considerations
The power supply of the pump has wide ranging capabilities and accepts any line voltage in the range mentioned in Table 2. Consequently, there is no voltage selector at the back of the instrument. There are also no externally accessible fuses, as automatic electronic fuses are implemented in the power supply.
WA R N I N G
To disconnect the pump completely from line power, unplug the power cord. The power supply still uses some power, even if the power switch on the front panel is turned off.
WA R N I N G
Shock hazard or damage of your instrumentation can result if the devices are connected to line voltage higher than specified.
CAUTION
Make sure to have easy access to the power cable of the instrument in order to disconnect the instrument from line.
Power Cords
Different power cords are offered as options with the pump. The female end of all power cords is identical. It plugs into the power-input socket at the back of the pump. The male end of each power cord is different and designed to match the wall socket of a particular country or region.
22
WA R N I N G
Never operate your instrumentation from a power outlet that has no ground connection. Never use a power cord other than the Agilent Technologies power cord designed for your region.
WA R N I N G
Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
Bench Space
The pump dimensions and weight (see Table 2) allow you to place the module on almost any table or laboratory bench. It needs additional 2.5 cm (1.0 inches) of space on either side and approximately 8 cm (3.1 inches) in the rear for air circulation and electric connections. Should the bench carry a Agilent 1200 Series system, be sure it is designed to bear the weight of all modules. The pump must be operated horizontal position.
Environment
Your pump will work within the specifications at ambient temperature and relative humidity described in Table 2.
CAUTION
Do not store, ship or use your pump under conditions where temperature fluctuations could cause condensation within the pump. Condensation will damage the system electronics. If your pump has been shipped in cold weather, leave it in its box and allow it to warm up to room temperature slowly to avoid condensation.
NOTE
The G1312B pump is designed to operate in a typical electromagnetic environment (EN61326-1) where RF transmitters, such as mobile phones, should not be used in close proximity.
23
Physical Specifications
Table 2
Type Weight
Physical Specifications
Specification 15.5 kg (34 lbs) 180 345 435 mm (7 13.5 17 inches) 100 240 VAC, 10 % 50 or 60 Hz 5 % 160 VA 0 55 C (32 131 F) -40 70 C (-4 158 F) < 95%, at 25 40 C (77 104 F) Up to 2000 m (6500 ft) Up to 4600 m (14950 ft) Installation category II, pollution degree 2 storage conditions Non-condensing Maximum . Wide-ranging capability Comments
Dimensions (width depth height) Line voltage Line frequency Power consumption (G1312B) Ambient operating temperature Ambient non-operating temperature Humidity Operating altitude Non-operating altitude Safety standards: IEC, CSA, UL, EN
24
Performance Specifications
Table 3
Type
Hydraulic system
Setable flow range Flow range Flow precision Flow accuracy Pressure Pressure pulsation
High-pressure binary mixing Standard delay volume configuration: 600-800 l, dependent on back pressure (includes 400 l mixer) Low delay volume configuration: 120 l measured with water
25
Table 3
Type
Performance Specifications of the Agilent 1200 Series Binary Pump SL, continued
Specification settable range: 0 100% recommended range: 1 99% or 5 l/min per channel, whatever is greater < 0.15 % RSD at 1mL/min Comments
Composition range
Composition precision
0.35% absolute Agilent ChemStation for LC (32-bit) G4208A Handheld Controller EZ Chrom Elite For pressure monitoring, 1.33 mV/bar, one output Controller-area network (CAN), RS-232C, APG Remote: ready, start, stop and shut-down signals, LAN optional Extensive diagnostics, error detection and display (through Agilent LC Diagnostics), leak detection, safe leak handling, leak output signal for shutdown of pumping system. Low voltages in major maintenance areas. Early maintenance feedback (EMF) for continuous tracking of instrument usage in terms of seal wear and volume of pumped mobile phase with pre-defined and user-settable limits and feedback messages. Electronic records of maintenance and errors. All materials recyclable.
GLP features
Housing
26
NOTE
For use with flow rates below 500 l/min or for use without damper and mixer a vacuum degasser is required. All specification measurements are done with degassed solvents.
27
28
This chapter gives information about the preferred stack setup for your system and the installation of your Binary Pump SL.
Agilent Technologies
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Damaged Packaging
When you receive your Binary Pump SL inspect the shipping boxes for any signs of damage. If the containers or cushioning material are damaged, save them until the contents have been checked for completeness and the pump has been mechanically and electrically checked. If the shipping container or cushioning material is damaged, notify the carrier and save the shipping material for inspection by the carrier.
CAUTION
If there are signs of damage to the pump, please do not attempt to install the instrument.
Delivery Checklist
Compare the delivery checklist with the contents of the shipping boxes to ensure completeness of the shipment. The contents lists is shown in Table 4. For parts identification check the illustrated parts breakdown in Chapter 9, Parts and Materials for Maintenance. Please report missing or damaged parts to your local Agilent Technologies sales and service office. Table 4
Description Binary Pump SL Calibration capillary assembly Agilent LC Diagnostic CD-ROM 1200 Binary Pump SL Start up Kit Syringe adapter luer/barb Syringe G1312-67500 G2173-64000 G1312-68700 0100-1681 9301-0411
Solvent cabinet (4 bottles, for pumps with solvent selection valve), or 5067-1531 Solvent cabinet (2 bottles, for pumps without solvent selection valve) 5067-1532
30
Table 4
Description
Solvent bottle amber Solvent bottle transparent Bottle head assembly 1200 Binary Pump SL User Manual SB-C18, 2.1x50mm,1.8um,600bar, or SB-C18, 4.6x50mm, 1.8um, 600bar, or Eclipse XDB-C18, 4.6x50mm, 1.8um, 600bar Power cable (matching your countrys power socket) Accessory kit (see Table 11)
31
If your Binary Pump SL is part of a complete Agilent 1200 series Rapid Resolution LC System, system performance can be optimized by stacking the instrument modules in either of the ways shown below.
32
Binary pump SL
Instant Pilot
Thermostat
Figure 5
NOTE
For a detailed view of the flow connections refer to the section Flow connections in the Rapid Resolution LC System manual.
33
RS232 connector, for factory use only CAN bus cable to Instant Pilot
G13 7 9 B M
C I RO
DE G A S E R S ( 2 5 0 V ) P O WE R M A X
WA R N I N G :
50 0 m
AC power cord
SE M ANUAL E
3 0W
T OA V OD I
E L C T R C A L S HO C K E I C
DI CONNE C S T
A T E NT I N: T O N I S T R U ME N T F O R M P O W P OU R E VI E R L E T S CHOS C R E S P P LY B E F RE U O
L E C T I QU E S E R
G 379 B 1
R E MOV I G C OER . N V C O U P E L A L I EN T A T O NA V A N T R M I
A DE
N I
J A P AN
CAN Bus cable for intermodule communication 5181-1516 (0.5m) 5161-1519 (1.0m)
Figure 6
34
NOTE
In order to optimize the flow path, the stacking order of the right stack is reversed. The sampler is located at the bottom and the detector is at the top.
Detector SL
Instant Pilot
Column Thermostat SL
Thermostat
Figure 7
35
LA N
Li nkC onf g i
I ni M ode t
V 1 00 - 1 20 / 20 - 2 40 2 H z 50 / 0 6 T 500 m A
30 W
( 250 V)
P OW ERM AX
G 1 37 9B
D E N L E V E R L C E COU V ER L E .
8 88 0 -
10
M A D I N JA PAN E
SEE MA NUAL
H I PB H - I Add r ss P B e
APG remote cable Pressure output to recorder, for PN of cable see page 64
Figure 8
36
Preparations
Locate bench space Provide power connections Unpack the pump Pump Power cord, for other cables see text below and Cable Overview on page 62 Agilent Control Software and/or Instant Pilot G4208A
Parts required
1 Place the Binary Pump SL horizontally on the bench. 2 Ensure the power switch on the front of the pump is OFF (switch stands out). 3 At the rear of the pump turn the security lever to expose the power inlet socket.
37
Status Indicator
Figure 9
4 Connect the power cable to the power connector at the back of the Binary Pump SL. The security lever prevents that the cover is opened while the power cord is connected to the pump. 5 Connect the required interface cables to the rear of the Binary Pump SL.
38
Configuration switch Slot for interface board RS232 Remote Analog output CAN-Bus
Figure 10
NOTE
In an Agilent 1200 Series system, the individual modules are connected through CAN cables. The Agilent 1200 Series vacuum degasser is an exception. It can be connected via APG remote connector to the other modules in the stack. An Agilent 1200 Series Instant Pilot can be connected to the CAN bus at any of the modules in the system except for the degasser. Connection to an Agilent data systems is established through an optional LAN board or the built-in LAN port (DAD SL). Although the LAN board can be installed into all modules except for the degasser and the Thermostatted Column Compartment, the LAN port of the detector should be used as the detector generates the highest data rate of all modules. In case the system comprises a G1315C DAD SL, it is mandatory to connect the data system to the LAN port of the DAD SL.For more information about connecting the Instant Pilot or Agilent Data System refer to the respective user manual. For connecting the Agilent 1200 Series equipment to non-Agilent equipment, see Chapter 15, Hardware Information in the Binary Pump SL Service Manual.
6 Connect the capillary, solvent tubes and waste tubings (see Flow Connections with Solvent Selection Valve on page 41 or Flow Connections
39
without Solvent Selection Valve on page 44). 7 Press the power switch to turn the pump on.
NOTE
The power switch stays pressed in and the green indicator LED in the power switch is on while the Binary Pump SL is turned on. When the line power switch stands out and the green light is off, the pump is turned off.
8 Purge the Binary Pump SL (see Priming the System on page 47).
WA R N I N G
To disconnect the Binary Pump SL from line power, unplug the power cord. The power supply still uses some power, even if the power switch on the front panel is turned off.
The pump is shipped with default configuration settings. To change these settings, see Setting the 8-bit Configuration Switch in the Binary Pump SL Service Manual.
40
WA R N I N G
When opening capillary or tube fittings, solvents may leak out. Please observe 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.
Pump is installed in the LC system Other modules Parts from accessory kit (see Cover Parts on page 147) Two wrenches 1/4 - 5/16 inch for capillary connections
1 Remove the front cover by pressing the snap fasteners on both sides.
41
Figure 11
2 If available, place the online degasser on top of the pump. 3 Place the solvent cabinet on top of the Binary Pump SL. 4 Set the four bottles into the solvent cabinet and screw a bottle head assembly onto each bottle. 5 Connect the solvent tubes from the bottle head assemblies to the inlet connectors A1, A2, B1 and B2 of the solvent selection valve. Make sure to use the brown bottle for the aqueous solvent (usually channel A1). 6 Label the tubes accordingly using the supplied stickers and fix the tubes in the clips of solvent cabinet and Binary Pump SL. 7 Hold the waste tubing with a piece of sandpaper and push it onto the purge valve outlet. Place the end into your waste system. 8 If the Binary Pump SL is not part of an Agilent 1200 Series system stack or placed at the bottom of a stack, connect the corrugated waste tube from the solvent leak drain of the pump to the leak handling system. 9 Connect the outlet capillary (pump to injection device) to the 1/4 inch Sawgelok outlet port of the purge valve. 10 Purge your system prior to the first use (see Priming the System on page 47).
42
Bottle-head assembly
Solvent cabinet
Degasser
Channel A1 Pressure sensor Static Mixer Purge valve Pump head B Pump head A Active inlet valve A Waste tubing Outlet capillary to autosampler Channel A2 Solvent selection valve Leak drain Channel B2 Active inlet valve B
Figure 12
43
WA R N I N G
When opening capillary or tube fittings, solvents may leak out. Please observe 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.
Pump is installed in the LC system Other modules Parts from accessory kit (see Cover Parts on page 147) Two wrenches 1/4 - 5/16 inch for capillary connections
1 Remove the front cover by pressing the snap fasteners on both sides.
44
Figure 13
2 Place the solvent cabinet on top of the Binary Pump SL. 3 Place the bottles into the solvent cabinet and place a bottle head assembly into each bottle. 4 Connect the solvent tubes from the bottle head assemblies to the inlet adapters of the active inlet valves. Fix the tubes in the clips of solvent cabinet and Binary Pump SL. 5 Hold the waste tubing with a piece of sandpaper and push it onto the purge valve outlet. Place the end into your waste system. 6 If the Binary Pump SL is not part of an Agilent1200 System stack or placed at the bottom of a stack, connect the corrugated waste tube from the solvent leak drain of the pump to the leak handling system. 7 Connect the outlet capillary (pump to injection device) to the 1/4 inch Sawgelok outlet port of the purge valve. 8 Purge your system before first use (see Priming the System on page 47).
45
Bottle-head assembly
Solvent cabinet
Tube clip (not visible) Degasser Pressure sensor Static Mixer Purge valve Pump head A Adapter Active inlet valve A Waste tubing Outlet capillary to autosampler Waste outlet Active inlet valve B Pump head B
Figure 14
46
Initial Priming
Purpose Before a new degasser or new solvent tubing can be used, it is necessary to prime the system. Isopropanol (IPA) is recommended as priming solvent due to its miscibility with nearly all HLPC solvents and its excellent wetting properties. Connect all modules hydraulically as described in the respective module manuals. Fill each solvent bottle with 100 mL isopropanol Switch the system on Isopropanol
Preparation
Parts required
NOTE
If the pump is not able to aspirate the solvent from the bottles, a syringe can be used to draw the solvent manually through tubing and degasser.
WA R N I N G
When opening capillary or tube fittings, solvents may leak out. Please observe 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.
NOTE
When priming the vacuum degasser with a syringe, the solvent is drawn through the degasser tubes very quickly. The solvent at the degasser outlet will therefore not be fully degassed. Pump for approximately 10 minutes at your desired flow rate before starting an analysis. This will allow the vacuum degasser to properly degas the solvent in the degasser tubes.
47
1 Open the purge valve of the pump 2 Set the flow rate to 5 mL/min. 3 Select channel A1 4 Turn the flow on 5 Observe if the solvent in the tubing of channel A1 is advancing towards the pump. If it isnt, disconnect the solvent tubing from the solvent selection valve, attach a syringe with a syringe adapter and pull the liquid through the degasser. Reattach the tubing to the solvent selection valve. 6 Pump 30 mL isopropanol to remove to remove residual air bubbles. 7 Switch to the next solvent channel and repeat steps 5 and 6 until all channels have been purged. 8 Turn the flow off and close the purge valve.
Regular Priming
Purpose When the pumping system has been turned off for a certain time (for example, overnight) air will rediffuse into the solvent channel between the vacuum degasser and the pump. Solvents containing volatile ingredients will slightly lose these if left in the degasser without flow for a prolonged period of time. Switch the system on none
1 Open the purge valve of your pump by turning it counterclockwise and set the flow rate to 5 mL/min. 2 Flush the vacuum degasser and all tubes with at least 10 mL of solvent. 3 Repeat step 1 and 2 for the other channel(s) of the Binary Pump SL. 4 Set the required composition and flow rate for your application and close the purge valve. 5 Pump for approximately 10 minutes before starting your application.
48
Changing Solvents
Purpose When the solvent of a channel is to be replaced by another solvent that is not compatible (solvents are immiscible or one solvent contains a buffer) it is necessary to follow the procedure below to prevent clogging of the pump by salt precipitation or residual liquid droplets in parts of the system. Remove the column and replace it by a ZDV fitting. Prepare bottles with appropriate intermediate solvents (see Table 5 on page 50) Purging solvent(s), see Table 5 on page 50
Preparation
Parts required
1 If the channel is not filled with a buffer, proceed to step 4. 2 Place the solvent intake filter into a bottle of water. 3 Flush the channel at a flow rate suitable for the installed tubing (typically 3-5 mL/min) for 10 min. 4 Modify the flow path of your system as required for your application. For delay volume optimization see the Rapid Resolution System manual. 5 Replace the solvent bottle by a bottle of isopropanol. 6 Flush the channel at a flow rate suitable for the installed tubing (typically 3-5 mL/min) for 5 min. 7 Swap the bottle of isopropanol with a bottle of solvent for your application.
CAUTION
Dont perform steps 5 to 7 if the solvent to be run is an aqueous buffer, because buffer salt may precipitate in residual isopropanol and clog the capillaries.
8 Repeat steps 1 to 7 for the other channel(s) of the Binary Pump SL. 9 Install the desired column, set the required composition and flow rate for your application and equilibrate the system for approx. 10 minutes prior to starting a run.
49
Table 5
Activity
After an installation
When switching between reverse phase and normal phase (both times) After an installation
Isopropanol
Ethanol or methanol
To clean the system when using buffers After changing aqueous solvents After the installation of normal phase seals (P/N 0905-1420)
50
This chapter explains the operational parameters of the Binary Pump SL.
Agilent Technologies
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Place solvent cabinet with the solvent bottles always on top (or at a higher level) of the Binary Pump SL. When using the Binary Pump SL without vacuum degasser, shortly degas your solvents (for example, water vacuum pump for 15 30 s in an appropriate vessel) before using them in the pump. If possible apply solvent conditions that will decrease the gas solubility over time (for example, warming up the solvents). The use of a vacuum degasser is mandatory for flow rates below 0.5 mL/min and for configurations without damper and mixer. When using the binary pump with vacuum degasser, flush the degasser with at least 5 mL per channel before operating the Binary Pump SL, especially when the pumping system had been turned off for a certain length of time (for example, overnight) and volatile solvent mixtures are used in the channels (see Regular Priming on page 48). Prevent blocking of solvent inlet filters (never use the pump without solvent inlet filters). Growth of algae should be avoided (see Prevent Blocking of Solvent Filters on page 70). Check purge valve frit and column frit in regular time intervals. A blocked purge valve frit can be identified by black, yellow or greenish layers on its surface or by a pressure greater than 10 bar when pumping distilled water at a rate of 5 ml/min with an open purge valve. Whenever possible use a minimum flow rate of 5 l/min per solvent channel to avoid crossflow of solvent into the unused pump channel. Whenever exchanging the pump seals, the purge valve frit should be exchanged, too. When using buffer solutions, flush the system with water before switching it off. The seal wash option should be used when buffer solutions with concentrations of 0.1 M or higher are being pumped for long periods of time. Check the pump plungers for scratches, grooves and dents when changing the piston seals. Damaged plungers cause micro leaks and will decrease the lifetime of the seals.
52
After changing the plunger seals, apply the seal wear-in procedure (see page 107). Place the aqueous solvent on channel A and the organic solvent on channel B. The default compressibility settings are set accordingly.
53
Solvent Information
Always filter solvents through 0.4 m 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 to 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 removed 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.
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Generic operation of the G4208A Instant Pilot is covered in the Instant Pilot Users Guide, part number G4208-90000. Details about setting up module specific parameters can be found in the Instant Pilot online help. The pump parameters are described in depth in Setting the Pump up with Agilent ChemStation on page 56
55
Overview
The pump parameters are grouped into six different panels: Set up Pump More Pump Auxiliary Data Curves Bottle Filling Contacts Control Most of these panels can be accessed in two different ways: Pulling down the Instrument menu or left-clicking on the pump icon the GUI.
Figure 15
56
Figure 16
57
Solvent type
Solvent comment
Figure 17 Table 6
Parameter Flow Stop Time Post Time
58
Table 6
Parameter Pressure Limits
Display
59
Pump Control
This panel is used to turn the pump on and off, operate the optional seal wash pump and define an error method. It can be accessed via menu Instrument - More Pump - Control or by left-clicking the pump icon in the GUI.
Figure 18
Pump
The pump group enables you to switch the pump On, Off or to Standby. In Standby, the pump motor is still energized. When the pump is switched on again, it does not re-initialize.
CAUTION
Upon initialization, the pump ignores the Maximum Flow Gradient value (see page 62). This can result in a rapid and uncontrolled pressure increase. To prevent harm to the column, open the purge valve until the initialization is finished.
60
Figure 19
61
Table 7
Parameter Maximum Flow Gradient Limits 0.1 - 100 mL/min
With this parameter flow rate changes can be ramped up and down slowly to avoid pressure shocks to the column. The default value is 100 ml/min2 which in fact turns the function off. Caution! The flow is shut off immediately when the pump switched to standby. When the pump is turned On from the Off status, the pump drive initializes, thereby ignoring the maximum flow gradient setting. Depending on system delay volume and flow restriction, the system pressure may rise very quickly to a high value. To protect your column from damage, it is suggested to open the purge valve during initialization. The volume one pump piston delivers per stroke. Generally, a smaller stroke volume results in lower pump ripple. The Auto setting adjusts the strokes dynamically to the lowest possible value. The strokes can be set individually for pump heads A and B. It is highly recommended to tick the Use enhanced compressibility calibration box. This forces the pump to use either stored solvent compressibility data or user generated compressibility parameters from solvent compressibility calibrations. For legacy support, the solvent compressibility can still be set manually for each channel when the box is unticked.
Minimum Stroke
Compressibility 0 - 150 E10-6/bar or enhanced compressibility calibration default: use enhanced comp. calibration
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Data Curves
The Binary Pump SL provides the possibility to store operational data in the data file of the Agilent data system. Solvent percentage for each channel, pump flow and pressure are stored when the respective boxes are ticked. Access the Data Curves panel either from the Instrument - More Pump - Data Curves menu or by left-clicking the pump icon in the GUI.
Figure 20
NOTE
The pressure data curve is generated from the pressure sensor readings, while %A, %B and flow are calculated from the method settings of the pump.
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Bottle Filling
The pump offers a powerful feature to monitor the liquid level in the solvent bottles. With total bottle volume and initial filling volume set correctly, the pump subtracts the displaced volume continuously from the initial value and reacts before the system runs dry or an analysis is corrupted. The Bottle Filling panel can be found in Instrument - More Pump - Bottle Filling or by left-clicking on the solvent bottles below the pump icon in the GUI.
Figure 21 Table 8
Parameter Total Volume Actual Volume Limits 0 - 1000 L default: 0 L 0 - 1000 L default: 0 L
64
Description When ticked, the pump wont start a new run if the solvent level in one or more bottles is below the given value. When setting this parameter, consider the size and shape of the solvent vessel and make sure the pump does not draw air when coming close to the limit. When ticked, the pump will turn off before air is aspirated. However, the residual solvent volume has been calculated for 1 L solvent bottles and may be too small for large bottles or other vessels.
CAUTION
The bottle filling feature will fail if multiple channels are fed from one solvent bottle! In that case implement a minimum pressure limit (see page 59) to avoid that the Binary Pump SL runs dry when solvents are empty,
65
Maintenance requires the exchange of components in the flow path which are subject to mechanical wear or stress. Ideally, the frequency at which components are exchanged should be based on the intensity of usage of the instrument and the analytical conditions, and not on a predefined time interval. The early maintenance feedback (EMF) feature monitors the usage of specific components in the instrument, and provides feedback when the user-settable limits have been exceeded. The visual feedback in the user interface provides an indication that maintenance procedures should be scheduled.
EMF Counters
The binary pump provides a series of EMF counters for the left and right pump heads. Each counter increments with pump use, and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded. Each counter can be reset to zero after maintenance has been done. The binary pump provides the following EMF counters: liquimeter pump A, seal wear pump A, liquimeter pump B, and seal wear pump B.
Liquimeters
The liquimeters display the total volume of solvent pumped by the left and right pump heads since the last reset of the counters. Both liquimeters can be assigned an EMF (maximum) limit. When the limit is exceeded, the EMF flag in the user interface is displayed.
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68
5 Optimizing Performance
Prevent Blocking of Solvent Filters 70 When to Use a Vacuum Degasser 72 When to Use the Active Seal Wash Option 73 When to Use Alternative Seals 74 When to Remove Damper and Mixer 75 How to Optimize the Compressibility Compensation Setting 78
This chapter gives information on how to optimize the performance of the Binary Pump SL under special operational conditions.
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Optimizing Performance
Contaminated solvents or algae growth in the solvent bottle will reduce the lifetime of the solvent filter and will influence the performance of the Binary Pump SL. This is especially true for aqueous solvents or phosphate buffers (pH 4 to 7). The following suggestions will prolong lifetime of the solvent filters and maintain the performance of the Binary Pump SL. Use a sterile, if possible amber, solvent bottle to slow down algae growth. Filter solvents through filters or membranes that remove algae. Exchange aqueous solvents every two days or refilter. If the application permits, add 0.0001 to 0.001 Molar sodium azide to the solvent. Place a layer of argon on top of your solvent. Avoid exposure of the solvent bottles to direct sunlight.
WA R N I N G
When opening capillary or tube fittings, solvents may leak out.Please observe 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.
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Optimizing Performance
NOTE
71
Optimizing Performance
The Binary Pump SL does not necessarily require degassing. However, for the following conditions a vacuum degasser is mandatory: Your detector is used with maximum sensitivity in the low UV wavelength range, Your application requires highest injection precision, or Your application requires highest retention-time reproducibility (flow rates below 0.5 mL/min). The Binary Pump SL is used with bypassed damper and mixer.
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Optimizing Performance
Concentrated buffer solutions will reduce the lifetime of the seals and plungers in your Binary Pump SL. The active seal wash option allows to maintain the seal lifetime by flushing the low pressure side of the seals with a wash solvent. The seal wash option is strongly recommended if buffer concentrations of 0.1 M or higher are used regularly with the Binary Pump SL. The active seal wash option kit can be ordered by quoting part number G1312-68712. The seal wash option comprises a peristaltic pump, secondary seals, gaskets, seal keepers and tubing for both pump heads. A bottle of premixed water/isopropanol (90/10 vol%) is placed in the solvent cabinet and connected to the peristaltic pump as described in the technical note that comes with the active seal wash kit. Always use a mixture of HPLC-water (90 %) and isopropanol (10 %) as wash solvent. This mixture prevents bacteria growth in the wash bottle and reduces the surface tension of the water. The operation of the peristaltic pump can be controlled from the data system or the Instant Pilot.
NOTE
The Binary Pump SL comes with pre-installed seal wash capable support rings. When the user decides to use seal wash it is recommended to replace the secondary seals and gaskets by new ones to ensure tightness.
For information on the installation of the continuous seal wash option refer to Installing the Active Seal Wash Option on page 126.
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Optimizing Performance
The standard seals for the Binary Pump SL can be used for most applications. However, normal phase applications (for example, hexane) are not compatible with the standard seals. They cause extremely high abrasion and significantly shorten seal life time. Special polyethylene pistons seals (yellow color), part number 0905-1420 (pack of 2). These seals have less abrasion compared to the standard seals.
NOTE
Polyethylene seals have a limited pressure range of 0200 bar. When used above 200 bar, their lifetime will be significantly reduced.
WA R N I N G
DO NOT apply the seal wear-in procedure performed to normal phase seals (yellow) because they will be destroyed by the procedure.
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Optimizing Performance
The Binary Pump SL is equipped with a pressure pulsation damper and a static mixer. The total delay volume of the pump is 600 800 L (depending on system pressure). The mixer has a volume of 400 L. For applications that require lowest delay volume (e.g. fast gradient methods or gradient applications with low flow rates), damper and mixer can be bypassed. (see Figure 22)
Standard configuration
Figure 22
Both configurations have advantages and weaknesses. For use with Agilent 1200 Series Rapid Resolution System check the System Configuration Optimizer on the CD-ROM that shipped with the pump for detailed plumbing recommendations for your application.
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Optimizing Performance
Preparations for this Flush the system (water if buffers were used, otherwise IPA). procedure Turn the flow off.
1 Remove the front cover by pressing the clip fastener on both sides of the cover.
2 Use the 1/4 inch hex driver to remove fitting B from port 2 of the pressure sensor.
A B 2 1
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Optimizing Performance
3 Fold capillary end B away. It remains unconnected. Disconnect fitting A from outlet 1 of the mixer.
4 Connect fitting A to port 2 of the pressure sensor. Seal port 1 of the mixer with a plastic blank nut.
A A 2 B 1 2 B 1
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Optimizing Performance
When a solvent is metered at ambient pressure and compressed to a higher pressure, the volume decreases. This is due to an effect known as solvent compressibility. Solvent compressibility is a non-linear function of pressure and temperature. It is unique to every solvent. In order to deliver the desired flow accurately at all pressures, Agilent pumps use a compressibility compensation. Usually, an average compressibility value for the solvent is used across the whole pressure range of the pump. The G1312B Binary Pump SL introduces a new compressibility compensation concept. The compressibility of a solvent is determined at different pressures between 0 to 600 bar. The pump uses the obtained non-linear function to select the correct compressibility value for the actual pump pressure. Compressibility data for the most common solvents is readily available in the pump firmware. The compensation algorithm is so powerful that the damper and mixer can be removed from the pump flow path at low flow rate while the pressure ripple and composition ripple remain at low levels. For method compatibility reasons, the legacy compressibility compensation is still available.
78
Optimizing Performance
79
Optimizing Performance
Table 9
Solvent Compressibility
Compressibility (10-6/bar) 126 115 95 110 100 118 114 104 120 150 100 100 120 100 87 46
Solvent (pure) Acetone Acetonitrile Benzene Carbon tetrachloride Chloroform Cyclohexane Ethanol Ethyl acetate Heptane Hexane Isobutanol Isopropanol Methanol 1-Propanol Toluene Water
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This chapter explains all test functions that are available for the Binary Pump SL.
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Pressure Test
Description
The pressure test is a quick built-in test designed to demonstrate the leak tightness of the system. The test involves monitoring the flow profile while the Binary Pump SL delivers against a blank nut. The result is presented as the leak rate of the pump and provides information about the leak tightness of the system between the outlet ball valves of the Binary Pump SL and the blank nut.
NOTE
The blank nut can be positioned anywhere between the purge valve of the pump and the detector inlet to pressure test the desired part of the system.
CAUTION
Never include the flow cell in the pressure test as the applied pressure may cause permanent leaks or bursting (FLD, RID) of the flow cell.
Step 1
The test begins with the initialization of both pump heads. After initialization, the pump is starting the compression phase and the required flow rate is constantly monitored and adjusted. The Binary Pump SL continues to pump until a system pressure of around 600 bar is reached.
Step 2
When the system pressure reaches 600 bar, the Binary Pump SL continues to pump at a flow rate that keeps the pressure constant. The flow that is needed to keep the pressure constant is directly translated into a leak rate.
82
If a specific component is suspected to cause the system leak, place the blank nut immediately in front of the suspected component, and run the pressure test again. If the test passes, the defective component is located behind the blank nut. Confirm the diagnosis by placing the blank nut immediately behind the suspected component. The diagnosis is confirmed if the test fails.
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Tools required
Preparations for this Place two bottles of HPLC-grade water in channels A and B (A1 and B1 if the procedure pump is equipped with a solvent selection valve)
NOTE
Make absolutely sure that all parts of the flow path that are part of the test are very thoroughly flushed with water before starting to pressurize the system! Any trace of other solvents or the smallest air bubble inside the flow path definitely will cause the test to fail!
NOTE
Make sure to release the pressure by opening the purge valve when the test has finished completed. Otherwise the pump may generate an overpressure error.
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NOTE
Please notice the difference between an error in the test and a failure of the test! An error is caused by the abnormal termination during the operation of the test whereas a failure of a test indicates that the test results were not within the specified limits.
If the pressure test fails: Ensure all fittings between the pump and the blank nut are tight. Repeat the pressure test.
NOTE
Often it is only a damaged blank nut itself (poorly shaped from overtightening) that causes the test to fail. Before investigating on any other possible sources of failure make sure that the blank nut you are using is in good condition and properly tightened!
If the test fails again, insert the blank nut at the outlet of the previous module in the stack (e.g. autosampler, port 6 of the injection valve), and repeat the pressure test. Exclude each module one by one to determine which module is leaking. If the pump is determined to be the source of the leak, run the pump test to identify the defective pump component.
Table 1
Potential Cause (Pump) Purge valve open. Corrective Action Close the purge valve.
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Table 1
Loose or leaky fitting. Damaged pump seals or plungers. Loose purge valve. Tighten the fitting or exchange the capillary. Run the pump test to identify the defective component. Tighten the purge valve nut (14 mm wrench).
Table 2
Potential Cause (Autosampler) Loose or leaky fitting. Rotor seal (injection valve). Damaged metering seal or plunger. Needle seat. Corrective Action Tighten or exchange the fitting or capillary. Exchange the rotor seal. Exchange the metering seal. Check the plunger for scratches. Exchange the plunger if required. Exchange the needle seat.
Table 3
Potential Cause (Column Compartment) Loose or leaky fitting. Rotor seal (column switching valve). Corrective Action Tighten or exchange the fitting or capillary. Exchange the rotor seal.
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Pump Test
Description
The pump test provides a fast and accurate way to verify proper hydraulic operation of the Binary Pump SL. Problems related to defective valves, seals or pistons can be diagnosed and usually the defective part is identified.
Step 1
The system is setup with water on both channels and a restriction capillary is attached to the outlet of the pump. Pump head A is delivering at 1 mL/min. The pressure signal is monitored and overlaid with the piston movement plot. The pressure pattern and the slope of the pressure signal are evaluated for the delivery strokes of both pistons.
Step 2
The procedure from step 1 is repeated on pump head B.
Step 3
The data from step 1 and 2 are evaluated. In case test failed, a conclusion about the defective part is made.
87
Tools required
Preparations for this Place two bottles of HPLC-grade water in channels A and B (A1 and B1 if the procedure pump is equipped with a solvent selection valve)
NOTE
Make absolutely sure that the pump is very thoroughly flushed with water before starting the test! Any trace of other solvents or the smallest air bubble inside the flow path definitely will cause the test to generate misleading results!
NOTE
Make sure to release the pressure by opening the purge valve when the test is completed. Otherwise the pump may generate an overpressure error.
88
Description
Each solvent or solvent mixture has unique compressibility at different pressures. In order to deliver accurate flow with minimal pressure- and composition ripple over the full operational pressure range, it is necessary that the Binary Pump SL compensates precisely for the compressibility of the solvents in use. The Binary Pump SL comes with compressibility parameters for the most common HPLC solvents and solvent mixtures. If a solvent is not available in the list of pre-calibrated solvents, the solvent compressibility calibration allows to generate appropriate compressibility data.
Technical background
The solvent compressibility calibration relies on an accurate elasticity calibration of the pump. With a proper elasticity calibration in place, the pump is switched into pressure control mode. A restriction capillary is connected to the purge valve outlet. By varying the flow rate, the pump maintains a certain pressure. The pump optimizes the compressibility value of the solvent until the lowest possible pump ripple is reached. The pump increases the flow rate and adjusts the pressure to the next calibration step where the pump ripple is minimized again. This process is repeated until solvent compressibility data for the whole operating pressure range of the pump are available. The compressibility data set for this solvent is stored in an XML-file and can be shared with other G1312B pump via Agilent ChemStation.
89
Tools required
Preparations for this Place a bottles with solvent to be calibrated in channel A (resp. A1 if a solvent procedure selection valve is installed).
CAUTION
Accurate pump elasticity calibration is required to obtain valid and portable solvent compressibility data.
NOTE
Make absolutely sure that the pump is very thoroughly flushed with the solvent to be calibrated before starting the procedure! Any trace of other solvents or the smallest air bubble inside the flow path definitely will cause the calibration to fail!
Running the Solvent Compressibility Calibration from the Agilent LC Diagnostic Software
1 Select the solvent from the test selection menu. 2 Start the test and follow the instructions.
NOTE
Make sure to release the pressure by opening the purge valve when the test is completed. Otherwise the pump may generate an overpressure error.
90
Description
The flow path components of the Binary Pump SL pump have an inherent and pressure dependent elasticity which differs from pump to pump. When this elasticity/pressure function is known, a correction algorithm can be applied. This results in significantly improved pump performance in low delay volume mode (damper and mixer bypassed). The pump elasticity calibration uses a solvent with well known properties (HPLC-grade water) to determine the pump elasticity over the entire operating pressure range and stores the calibration values in the non-volatile RAM of the pump mainboard. The initial calibration is done at the factory. It only needs to be repeated after replacement of major pump parts (mainboard, pump drive). The test allows to define which pump head will be calibrated.
NOTE
Results of the pump elasticity calibration rely on known compressibility parameters for pure water. If the water is not HPLC-grade, not well degassed or degasser and pump are not flushed properly, the pump elasticity calibration will fail. The pump elasticity calibration has to be performed for each pump head individually.
CAUTION
Missing or inaccurate pump elasticity calibration will result in a wrong solvent compressibility calibration (see page 89) parameters
91
Preparations for this Place all bottle heads in to a bottle of HPLC-grade water. procedure
NOTE
Make absolutely sure that the pump is very thoroughly flushed with the solvent to be calibrated before starting the procedure! Any trace of other solvents or the smallest air bubble inside the flow path definitely will cause the calibration to fail!
NOTE
If a solvent selection valve is installed flush all four solvent channels to avoid that air from a dry solvent intake tube is drawn into the flow path upon initialization.
Running the Pump Elasticity Calibration from the Agilent LC Diagnostic Software
1 Select the pump elasticity calibration from the test selection menu. 2 Start the test and follow the instructions.
92
This chapter provides general information on repairing the Binary Pump SL.
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94
WA R N I N G
To prevent personal injury, the power cable must be removed from the instrument before opening the pump cover. Do not connect the power cable to the pump while the covers are removed.
WA R N I N G
To prevent personal injury, be careful when getting in contact with sharp metal areas.
WA R N I N G
When working with solvents please observe 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.
CAUTION
Electronic boards and components are sensitive to electrostatic discharge (ESD). In order to prevent damage always use an ESD protection when handling electronic boards and components (see Using the ESD Strap on page 97).
95
The pump case should be kept clean. Cleaning should be done with a soft cloth slightly dampened with water or a solution of water and mild detergent. Do not use an excessively damp cloth as liquid may drip into the pump.
WA R N I N G
Do not let liquid drip into the pump. It could cause shock hazard and it could damage the module.
96
Electronic boards are sensitive to electrostatic discharge (ESD). In order to prevent damage, always use an ESD strap when handling electronic boards and components. 1 Unwrap the first two folds of the band and wrap the exposed adhesive side firmly around your wrist. 2 Unroll the rest of the band and peel the liner from the copper foil at the opposite end. 3 Attach the copper foil to a convenient and exposed electrical ground.
Figure 1
97
98
This chapter describes all maintenance and simple repair procedures that can be performed without removing the pump from the system stack.
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Figure 2 shows the main user accessible assemblies of the Binary Pump SL. The pump heads and its parts do require normal maintenance (for example, seal exchange) and can be accessed from the front (simple repairs). Replacement of valve cartridges or filters dont require to remove the pump from the system stack.
Delay volume reduction Seal wash option, see page 126 Outlet ball valve, see page 121 Pump head, see page 104 Active inlet valve, see page 116
Figure 2
100
Maintenance Procedures
The procedures described in this section can be done with the Binary Pump SL in place in the system stack. Table 1
Procedure Exchanging the Purge Valve Frit or the Purge Valve on page 102
Maintenance Procedures
Typical Frequency Yearly, or if the frit shows indication of contamination or blockage During yearly maintenance Notes A pressure drop of > 10 bar across the frit (5 mL/min H2O with purge valve open) indicates blockage Necessary to get access to pump seals and plungers. Necessary to get access to pump seals and plungers. Leaks at lower pump head side, unstable retention times, pressure ripple unstable run pump test for verification Seal life time shorter than normally expected check plungers while changing the seals Only necessary when Seal Wash Option is installed. Leaks at lower pump head side, loss of wash solvent
Disassembling the pump head on page 106 During yearly maintenance Exchanging the Pump Seals on page 107 Yearly, or if pump performance indicates seal wear If scratched or if dents are visible Yearly
101
Tools required
Parts required
1 Using a 1/4 inch wrench disconnect the pump outlet capillary at the purge valve. 2 Disconnect the waste tube. Beware of leaking solvents due to hydrostatic pressure. 3 Using the 14 mm wrench, unscrew the purge valve and remove it from the purge valve holder. 4 Remove the plastic cap with the gold seal from the purge valve. 5 Use a pair of tweezers or a toothpick to remove the frit.
Valve body
Figure 3
102
6 Place a new frit into the purge valve with the slit facing the gold seal (see Figure 3). 7 Replace the cap with the gold seal.
NOTE
Before reinstallation always check the gold seal. A deformed seal or a cracked cap should be replaced.
8 Insert the purge valve into the purge valve holder and orient he waste outlet nozzle downward as shown below. 9 Tighten the purge valve and reconnect outlet capillary and waste tubing.
Purge valve
Waste tube
Figure 4
103
NOTE
Both pump head assemblies use the same internal components. In addition, pump head A is fitted with the purge valve. The following procedure describes the removal and disassembly of pump head A (left). For pump head B (right) proceed in the same way and skip steps that deal with the purge valve.
When required
Exchanging pump seals Exchanging plungers Exchanging seals of the seal wash option Wrench 1/4 inch 3-mm hexagonal key 4-mm hexagonal key 1/4 inch slitted socket wrench
Tools required
Preparations for this Switch off the Binary Pump SL at power switch procedure
1 Remove the front cover. 2 Disconnect the capillary at the pump head adapter and the tube at the active inlet valve. Beware of leaking solvents. 3 Using a 3-mm hexagonal key loosen the purge valve holder and lift it up. 4 Disconnect the active inlet valve cable. 5 Using a 4-mm hexagonal key stepwise loosen and remove the two pump head screws
104
Figure 5
105
106
Parts required
Preparations for this Switch off Binary Pump SL at power switch procedure Remove the front cover to have access to the pump mechanics Removing the Pump Head Assembly on page 104
1 Disassemble the pump head assembly, seeDisassembling the pump head on page 106. 2 Use one of the plungers to carefully remove the seal from the pump head (be careful not to break the plunger).
Plunger
Pump seal
Pump head
Figure 6
107
3 Insert seals into the pump head and press firmly in position.
Pump seals
Figure 7
4 Reassemble the pump head assembly (see Reinstalling the Pump Head Assembly on page 113).
NOTE
Reset the seal wear counter and liquimeter with the in the Agilent LC Diagnostic software.
108
1 Put a bottle with 100 ml of isopropanol in the solvent cabinet and place the solvent intake filter of the pump head you want to wear in into this bottle. 2 Screw the PEEK adapter (part no. 0100-1847) onto the Active Inlet Valve and connect the inlet tube directly to it. 3 Connect the restriction capillary (part no. 5022-2159) to the purge valve. Put its other end into a waste container. 4 Open the purge valve and purge the system for 5 minutes with isopropanol at a flow rate of 2 mL/min. 5 Close the purge valve, set the flow to a value that gives a pressure of 350 bar. Pump 15 minutes at this pressure to wear the seals in. The pressure can be monitored on the analog output connector of the pump, with the Instant Pilot, Chemstation or any other controlling device connected to your pump. 6 Turn the pump Off, slowly open the purge valve to release the pressure from the system, disconnect the restriction capillary and reconnect the outlet capillary to the purge valve. Reconnect the intake tubing to the solvent selection valve and the connecting tube from solvent selection valve (if installed) to the AIV. 7 Purge your system with the solvent used for your next application.
109
Parts required
Preparations for this Switch off Binary Pump SL at power switch procedure Remove the front cover to have access to the pump mechanics Removing the Pump Head Assembly on page 104 Disassembling the pump head on page 106
1 Check the plunger surface and remove any deposits or layers. Most suitable is polishing of the plunger rod with toothpaste. Replace the plunger if scratched of if dents are visible.
NOTE
The best way to inspect a piston is to hold it up and watch e.g. a light bulb though the piston rod. The transparent sapphire acts as a very strong magnifier and even smallest surface abnormalities become visible.
Figure 8
Plunger
110
Parts required
Preparations for this Switch off Binary Pump SL at power switch procedure Remove the front cover to have access to the pump mechanics Removing the Pump Head Assembly on page 104 Disassembling the pump head on page 106
1 Remove the seal keeper and the seal wash support rings from the plunger housing. Remove the seal keeper from the support ring assembly. Seal keeper Seal wash support ring
2 Using the blade of a flat head screwdriver remove seal wash gasket and the secondary seal from the support ring.
Plunger
Support ring
111
3 Using the insert tool press the seal (spring pointing upwards) into the recess of the support ring. Place a seal wash gasket in the recess of the support ring and replace the seal keeper.
4 Reassemble the pump head assembly (see Reinstalling the Pump Head Assembly on page 113).
Insert tool
112
Parts required
2 Using a 4 mm hexagonal key tighten the pump head screws stepwise with increasing torque. 3 Using a 3 mm hexagonal key fix the purge valve holder to the pump head. 4 Reconnect the capillaries, tubing and the active inlet valve cable to the connector.
113
Capillary to T-piece
Figure 9
114
The procedures described in this section can be done with the Binary Pump SL in place in the system stack. Table 2
Procedure Exchanging the Purge Valve Frit or the Purge Valve on page 102 Exchanging the Active Inlet Valve Cartridge on page 116 Exchanging the Active Inlet Valve Body on page 118 Exchanging the Outlet Ball Valve on page 121 Exchanging the Solvent Selection Valve on page 124 Installing the Active Seal Wash Option on page 126
115
Preparations for this Switch off Binary Pump SL at power switch procedure
1 Remove the front cover. 2 Unplug the active inlet valve cable from the connector. 3 Disconnect the solvent inlet tube at the inlet valve (beware of leaking solvents).
NOTE
Binary Pump SLs without the solvent selection valve (SSV) have an adapter installed between the solvent line and the active inlet valve (AIV). Disconnect the solvent tubes at the adapter and remove the adapter from the AIV.
4 Using a 14-mm wrench loosen the active inlet valve and remove the valve from the pump head. 5 With a pair of tweezers, remove the valve cartridge from the active inlet valve. 6 Clean the inside of the active inlet valve body. Flush the cartridge area thoroughly. 7 Push a new valve cartridge into the valve body. Make sure the valve cartridge is fully inserted. 8 Screw the valve into the pump head. Using the 14 mm wrench turn the nut until it is hand tight. 9 Position the valve so that the solvent inlet tube connection points towards the front. 10 Using the 14 mm wrench tighten the nut by turning the valve in its final position (do not overtighten the valve). 11 Reconnect the Active Inlet Valve cable to the connector in the Z-panel and the inlet tube to the valve.
116
NOTE
After an exchange of the valve it may be required to pump several mL of solvent before the flow stabilizes at a pressure ripple as low as it used to be when the system was still working properly.
Figure 10
117
Preparations for this Switch off Binary Pump SL at power switch procedure
1 Remove the front cover. 2 Unplug the active inlet valve cable from the connector. 3 Disconnect the solvent inlet tube at the inlet valve (beware of leaking solvents).
NOTE
Binary Pump SLs without the solvent selection valve (SSV) have an adapter installed between the solvent line and the active inlet valve (AIV). Disconnect the solvent tubes at the adapter and remove the adapter from the AIV.
4 Using a 14-mm wrench, loosen the active inlet valve and remove the valve from pump head.
118
Connector
Figure 11
5 Using a pair of tweezers, remove the valve cartridge from the defective active inlet valve. 6 Push the cartridge into the new active inlet valve.
Figure 12
7 Insert the new valve into the pump head. With the 14 mm wrench turn the nut until it is hand tight.
119
8 Position the valve so that the solvent inlet tube connection points towards the front. 9 Using the 14 mm wrench tighten the nut by turning the valve in its final position (not more than a quarter turn). Do not overtighten the valve.
WA R N I N G
Overtightening the active inlet valve will destroy the active inlet valve cartridge.
10 Reconnect the Active Inlet Valve cable to the connector in the Z-panel and the inlet tube to the valve. 11 Reinstall the front cover.
NOTE
After an exchange of the valve it may be required to pump several mL of the solvent used in the current application before the flow stabilizes at a pressure ripple as low as it used to be when the system was still working properly.
120
NOTE
Before exchanging the outlet ball valve you can try to clean it in an ultrasonic bath. Remove the gold seal and put the plastic cap back on to protect the sealing surface from scratches. Place the valve in upright position (sitting on the plastic cap) in a small beaker with premixed water/isopropanol (50/50). Sonicate for 5 to 10 minutes. Replace the gold seal.
1 Using a 1/4 inch wrench disconnect the valve capillary from the outlet ball valve. 2 Unscrew the valve with the 14 mm wrench and remove it from the pump body. 3 In case you are only sonicating the valve, check the plastic cap and the gold seal for damage.
NOTE
Check the gold seal. It should be exchanged when heavily deformed. Inspect the cap and replace it with a new one if cracks are visible.
121
Gold seal
Plastic cap
Figure 13
4 Reinstall the outlet ball valve and tighten it. 5 Reconnect the valve capillary.
122
Absorber capillary
Figure 14
123
1 Lift solvent bottle A1 out of the solvent cabinet and place it on the table. Disconnect the solvent tube from channel A1 (upper left) of the solvent selection valve and empty the tube into the bottle. Place the bottle back into the solvent cabinet. 2 Repeat step 1) for the remaining solvent channels. 3 Disconnect the active inlet valve connection tubes from the solvent selection valve. 4 Using a Pozidriv screwdriver #1 loosen the holding screws of the valves. 5 Pull the valve module out. 6 Hold the two plastic bodies of the valves and pull the two solvent selection valves apart. 7 Exchange the defective solvent selection valve. Join the new valve (new half) and the properly working old one. 8 Push the valve module into the cutout of the pump body until the electrical connectors are properly seated and fix the assembly with the two holding screws. 9 Reinstall solvent tubes and the active inlet valve connection tubes.
124
Figure 15
125
Preparations for this Switch off the pump at the main power switch procedure Remove the front cover Remove the top cover and foam
Figure 16
126
2 Insert the socket, delivered with the Seal Wash pump assembly, into the hole on the z-panel. 3 Guide the wire of the active seal wash assembly through the hole and screw it onto the z-panel. 4 Guide the wire over the fan and plug the connector onto the mainboard connector P7.
Figure 17
5 Replace the foam and top cover. 6 Disconnect all capillaries and tubes from the pump head and disconnect the active inlet valve cable. 7 Using a 4-mm hexagonal key stepwise loosen and remove the two pump head screws and remove the pump head from the pump drive 8 Place the pump head on a flat surface. Loosen the lock screw (two revolutions) and while holding the lower half of the assembly carefully pull the pump head away from the plunger housing.
127
Figure 18
9 Remove the support rings from the plunger housing and lift the housing away from the plungers. 10 Replace the seal wash seals and the film gaskets of the support rings.
128
Figure 19
11 Place the support rings on the plunger housing (plungers not installed) and snap the pump head and plunger housing together. 12 Insert the plungers and carefully press them into the seal. 13 Tighten the lock screw. 14 Slide the pump head assembly onto the metering drive. Apply a small amount of pump head grease (part no. 79846-65501) to the pump head
129
screws and the balls of the spindle drive. Tighten the pump head screws stepwise with increasing torque until they are tight. 15 Reconnect all capillaries, tubes and the active inlet valve cable to its connector 16 Route the wash tubings as shown in inlet tube into a bottle filled with a mixture of distilled water and isopropanol (90/10) and place the bottle in the solvent cabinet. 17 Route the outlet of the wash tube back into the wash solvent bottle.
Figure 20
130
CAUTION
The interface board is sensitive to electrostatic discharge. Always use the ESD kit when handling electronic boards.
Board defective
BCD (Interface) board, see Optional Interface Boards on page 152
1 Switch OFF the Binary Pump SL at the main power switch. Unplug the pump from main power. 2 Disconnect cables from the interface board connectors. 3 Loosen the screws. Slide out the interface board from the Binary Pump SL. 4 Install the new interface board. Secure screws. 5 Reconnect the cables to the board connector
131
BCD (Interface)
Figure 21
132
If a new version resolves problems of the currently installed version or if the firmware version of a new CSM board is different from the previous one. LAN/RS-232 Firmware Update Tool, or Instant Pilot G4208A Firmware, tools and documentation from Agilent web site Read update documentation provided with the Firmware Update Tool.
The installation of older firmware might be necessary: to keep all systems on the same (validated) revision, or if third part control software requires a special version. To upgrade/downgrade the pumpss firmware the following steps have to be performed: 1 Download the modules firmware, the LAN/RS-232 FW Update Tool version 2.1 or above and the documentation from the Agilent web site: http://www.chem.agilent.com/scripts/cag_firmware.asp. 2 Load the firmware into the pump as described in the documentation.
NOTE
The G1312B Binary Pump SL requires firmware revision A.06.02 or above (main and resident).
133
134
This chapter lists all parts and tools that are required for maintenance and simple repairs.
Agilent Technologies
135
Table 3
Item 1 2 3 4 5 6 7 8
136
4 3 5
1/2
7 8
Figure 22
137
Table 4
Item 1 2
4 5 6 7 8 9 10 11 12 13 14
Active inlet valve, see page 146 Pump head, see page 142 Outlet ball valve, see page 144 Absorber capillary Mixing capillary Restriction capillary (mixing capillary to pressure sensor) Pressure sensor Capillary SSL, 0.17 x 150 mm (pressure sensor to damper) Damper Solvent mixer Capillary SSL, 0.17 x 105 mm (connections to solvent mixer) Bracket for solvent mixer G1312-87300 G1312-67302 G1312-87301 see Service Manual G1312-87305 see Service Manual G1312-87330 G1312-87306 G1312-04100
15
Purge valve SL, see page 145 Peristaltic pump cartridge (silicone tubing), not shown Tubing, 1 mm ID, 3 mm OD, silicone, 5 m, for seal wash option 5042-8507 5065-9978
138
Table 4
Item 16
17
11 14
13
12 9
10 15 5 4 17 16 1 2 3 7 6
Figure 23
139
Table 5
Item 1 2 3 4 5 6 7 8 9 10 11 12 13
Hydraulic Path without Solvent Selection Valve, With Active Seal Wash
Description Solvent tubing, (kit of 4 ea. degasser to pump SSV) PEEK adapter 1/4-28 to 10-32 Active inlet valve, see page 146 Pump head, see page 142 Outlet ball valve, see page 144 Absorber capillary Mixing capillary Restriction capillary (mixing capillary to pressure sensor) Pressure sensor Capillary SSL, 0.17 x 150 mm (pressure sensor to damper) Damper Solvent mixer Capillary SSL, 0.17 x 105 mm (connections to solvent mixer) Bracket for solvent mixer G1312-87300 G1312-67302 G1312-87301 see Service Manual G1312-87305 see Service Manual G1312-87330 G1312-87306 G1312-04100 Part Number G1322-67300 0100-1847
14 15
Purge valve SL, see page 145 Capillary, pump to injector device (0.17 x 400 mm, SSL) Capillary, pump to thermostattable autosampler (0.17 x 700 mm, SSL) Waste tube, 5 m Peristaltic pump (silicone tubing) Tubing, 1 mm ID, 3 mm OD, silicone, 5 m, for seal wash option G1312-87303 G1312-87304 5062-2461 5042-8507 5065-9978
16 17 18
140
10 13
12
11 8
18
9 14 4
17 5 7
3 15
16
Figure 24
Hydraulic Path with Solvent Selection Valve, with Active Seal Wash
141
Pump-Head Assembly SL
Table 6
Item
Sapphire piston Lubricant, black (apply to piston base) Plunger housing (including springs) Support ring (includes wash seal) Wash seal Tubing for seal wash option (not shown) 1 mm ID, 3 mm OD, silicone, 5 m, Gasket, seal wash (pack of 6) Seal keeper (pack of 2) Seal (pack of 2) or Seal (pack of 2), for normal phase applications (optional) Absorber capillary Pump chamber housing Active inlet valve body (without cartridge) Replacement cartridge for active inlet valve SL Screw, purge-valve holder Purge-valve holder Outlet ball valve SL Screw lock Adapter Purge valve assembly SL Screw M5 60 mm lg
142
Table 6
Item 19 20
17 12 5 2 13 17 13 1
15
14 4 8 10 7
3 6
18
16
9 19 11 20
Figure 25
143
Table 7
Item
1 2 3 4
Housing screw Outlet valve cartridge Gold seal, outlet Cap (pack of 4, reorder number)
2 3 4
144
Table 8
Item
Purge-Valve Assembly
Description Purge valve SL complete assembly Part Number G1312-60023 No part number 01018-22707 5001-3707 5062-2485
1 2 3 4
Valve body PTFE frit (pack of 5) Gold seal Cap (pack of 4, reorder number)
2 3 4
Figure 26
Purge Valve
145
Table 9
Item 1 2
Valve body
2 Valve cartridge
Figure 27
146
Cover Parts
Table 10
Item 1
Cover Parts
Part Number G1312-68724
Figure 28
Cover Parts
147
Table 11
Description
Insert tool for wash seals PTFE Frit (pack of 5) PTFE tubing, 1.45 mm ID, length 2 m, purge valve to waste PTFE tubing, 1.45 mm ID, reorder (gives 5 m) Waste tubing assembly Corrugated waste tube, reorder, (gives 5 m) Hex key 4 mm, 15 cm long T-handle Wrench 1/4 5/16 inch Hex key 3 mm, 12 cm long Wrench, 14 mm Hex driver open, 1/4 inch CAN cable, 1 m long Capillary, pump to sampler, 400 mm lg, id 0.17 mm Capillary, pump to thermostatted sampler, 700 mm lg, id 0.17 mm
148
Table 12
Description
Seal wash pump assembly (includes peristaltic pump and pump motor) Peristaltic pump, silicone tubing Secondary seal (4 ea.) Gasket, wash seal (4 ea) (reorder gives pack of 6) Silicone rubber tubing 1mm I.D. (3m) Seal (2 packs of 2 for Binary Pump SL) Seal insertion tool
149
Table 13
Item * * * *
Description Carrier for Heater or Cooling Devices, QTY=2 High Temperature Heater (0.12 mm i.d. 1.6 l), QTY=1 High Temperature Heater (0.12 mm i.d. 1.6 l), QTY=1 Cooler (0.12 mm i.d. 1.5 l), QTY=1 Capillary System Kit, see Table 14 for details
For items * see also Heater and Cooler Devices for G1316B in the G1316B User Manual. Table 14
Item
Description Seat Capillary 100 mm x 0.12 mm, 0.8 OD DAD Heat Exchanger Capillary 310 mm x 0.12 mm SS Capillary 340 mm x 0.12 mm, m/m SS Capillary 300 mm x 0.12 mm, m/m SS Capillary 210 mm x 0.12 mm, m/m SS Capillary 170 mm x 0.12 mm, m/m SS Capillary 130 mm x 0.12 mm, m/f SS Capillary 90 mm x 0.12 mm, m/f SS Capillary 70 mm x 0.12 mm, m/f SS Capillary 50 mm x 0.12 mm, m/f SS Capillary 170 mm x 0.12 mm, m/f
150
Table 14
Item
Description SS Capillary 500 mm x 0.12 mm, m/m SS Capillary 500 mm x 0.12 mm, m/m
151
The Agilent 1200 Series modules have one optional board slot that allows to add an interface board to the modules. Table 15
Description BCD Board Fuse 250 mA (four are on the board LAN Communication Interface Board
152
A Appendix
General Safety Information 154 Lithium Batteries Information 157 Radio Interference 158 Sound Emission 159 Solvent Information 160 Agilent Technologies on the Internet 162
Agilent Technologies
153
Appendix
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.
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. The Agilent 1200 modules are designed and certified as a general purpose laboratory instrument for research and routine application only. It is not certified for in-vitro or medical applications.
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.
154
Appendix
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.
CAUTION
The operator of this instrument is advised that if the equipment is used in a manner not specified in this manual, the protection provided by the equipment may be impaired.
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 as much as possible. When inevitable, this should 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.
155
Appendix
Safety Symbols
Table 16 shows safety symbols used on the instrument and in the manuals. Table 16
Symbol
Safety Symbols
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.
WA R N I N G
A warning alerts you to situations that could cause physical injury or damage to the equipment. Do not proceed beyond a warning until you have fully understood and met the indicated conditions.
CAUTION
A caution alerts you to situations that could cause a possible loss of data. Do not proceed beyond a caution until you have fully understood and met the indicated conditions.
156
Appendix
WA R N I N G
Danger of explosion if battery is incorrectly replaced. Replace only with the same or equivalent type recommended by the equipment manufacturer. Lithium batteries may not be disposed-off into the domestic waste. Transportation of discharged Lithium batteries through carriers regulated by IATA/ICAO, ADR, RID, IMDG is not allowed. Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries.
WA R N I N G
Lithiumbatteri - Eksplosionsfare ved fejlagtig hndtering. Udskiftning m kun ske med batteri af samme fabrikat og type. Lever det brugte batteri tilbage til leverandren.
WA R N I N G
Lithiumbatteri - Eksplosionsfare. Ved udskiftning benyttes kun batteri som anbefalt av apparatfabrikanten. Brukt batteri returneres appararleverandoren.
NOTE
Bij dit apparaat zijn batterijen geleverd. Wanneer deze leeg zijn, moet u ze niet weggooien maar inleveren als KCA.
157
Appendix
Radio Interference
Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
158
Appendix
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)
159
Appendix
Solvent Information
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. If the flow cell is transported while temperatures are below 5 degree C, it must be assured that the cell is filled with alcohol. Aqueous solvents in the flow cell can built up algae. Therefore do not leave aqueous solvents sitting in the flow cell. Add small % of organic solvents (e.g. acetonitrile or methanol ~5%).
Solvents
Brown glass ware can avoid growth of algae. Always filter solvents through 0.4 m 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 acid 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.
160
Appendix
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.
161
Appendix
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 also provide the latest firmware of the Agilent 1200 series modules for download.
162
Index
Index
Numerics
0100-1681, 30 5041-2168, 136 5062-2483, 136 5062-8517, 136 5063-6598, 136 5063-6599, 136 5067-1531, 30 5067-1532, 30 827700-902, 31 827975-902, 31 927975-902, 31 9301-0411, 30 9301-1420, 31, 136 9301-1450, 31, 136
B
battery, 157 BCD board, 131 fuses, 152 output, 18 bench space, 23, 29 binary pump SLdelivery checklist, 30 blank nut, 1/16 inch, 84 bottle head assembly, 31, 136 inlet filter adapter, 136 solvent inlet filter, 136 solvent tubing, 136 tube screw, 136 bottles amber, 136 transparent, 136 buffer application, 52 buffer solutions, 12
compressibility calibration, 89 compressibility compensation, 25, 78 configuration low flow rates, 52 stacking, 32 connections flow, 41, 44 connector APG remote, 39 RS-232C, 18 control and data evaluation, 26 cover parts, 142, 147
D
damaged packaging, 30 damaged parts, 30 damper when to remove, 75 data evaluation and control, 26 delay volume, 14, 75 delivery checklist, 30 binary pump SL, 30 design, 13 detector signal, 36 dimensions and weight, 24 dual-piston in-series design, 13
A
accessory kit, 31, 147 active inlet valve, 116, 118, 146 active inlet valve body, 115 active seal wash, 73 Active seal wash, seal wash, active, 12 adapter, 45, 116, 118 inlet filter, 136 syringe luer/barb, 30 Agilent LC Diagnostic CD-ROM, 30 Agilent LC Diagnostic SW, 84 Agilent on internet, 162 algea, 52, 70, 160 alternative seal material, 74 amber bottle, 70 analog output, 18 analog pressure signal, 36 analog signal, 36 analog signal output, 26 APG remote cable, 36 APG remote connector, 39 assembly bottle head, 136 AUTO, pump stroke, 17
C
cable APG remote, 36 CAN, 36, 39 interface, 38 LAN, 36 power, 31 Calibration capillary assembly, 30 CAN bus, 18 CAN cable, 36, 39 capillary calibration, 30 CD-ROM Agilent LC Diagnostic, 30 column Eclipse XDB-C18, 4.6x50mm, 1.8um, 600bar, 31 SB-C18, 2.1x50mm,1.8um,600bar, 31 SB-C18, 4.6x50mm, 1.8um, 600bar, 31 compensation, compressibility, 25 composition precision, 26 composition ripple, 89
E
early maintenance feedback (EMF), 12 Eclipse XDB-C18, 4.6x50mm, 1.8um, 600bar, 31 electrical connections, 18 electronic fuses, 18 EMF, 12 EMF counters, 66 (maximum) limit, 66 liquimeter, 66 seal wear, 67 setting limits, 67 usage, 67 EMF flag, 66 EMF limits, 67 environment, 23 error messages
163
Index
overpressure, 84 ESD (electrostatic discharge) strap, 97 exchange active inlet valve, 116 Exchanging, 102, 111 exchanging active inlet valve, 115, 116, 118 interface board, 131 internal parts, 133 outlet ball valve, 115, 121 outlet ball valve sieve, 115, 121 pistons, 101, 110 pump seals, 101, 107 purge valve, 102, 115 purge valve frit, 102, 115 solvent selection valve, 124 wash seals, 101, 111, 126 external contacts, 18
frit, 102 front view, single stack, 33 front view, twin stack, 35 fuse, 18 fuses BCD board, 152
K
kit accessory, 31
G
G1311-60003, 136 G1312-67500, 30, 92 G1312-68700, 30 G131268725, 31 G1312-90010, 31 G2173-64000, 30 gas solubility, 52 gradient formation, 25
L
LAN cable, 36 leak parts, 142 line frequency, 18 line voltage, 18 Liquimeter, 66 liquimeter, 108 lithium battery, 157 low delay volume configuration, 75
F
features GLP, 26 instrument layout, 12 safety and maintenace, 26 ferrules with lock ring, 136 filter solvent inlet, 52 solvent inlet filter, 136 Filters prevent blockages, 70 filters algae, 70 firmware updates, 133 flow cell solvent information, 160 flow connections, 41, 44 flow path Low delay volume configuration, 75 Standard configuration, 75 flow precision, 25 flow range, 12 operational, 25 setable, 25 flow rate minimum, 52 foam parts, 142 frequency range, 18
H
hexagonal key 4 mm, 110, 111, 113 hexagonal key, 3 mm, 104, 107, 110, 111, 113 hexagonal key, 4 mm, 104, 107, 110, 111, 113 high-pressure mixing, 12 hints for successful use, 52 humidity, 24 hydraulic path with solvent selection valve, 138 hydraulic path without solvent selection valve, 140 hydraulic system, 25
M
main assemblies, overview, 100 maintenance replacing firmware, 133 maintenance procedures, 66 minimum flow rate, 52 missing parts, 30 mixer, 13 when to remove, 75
O
operating altitude, 24 operation temperature, 24 outlet ball valve, 115, 121, 144 overpressure error, 84
I
injection precision, 72 inlet filter adapter, 136 insert tool, 111, 113 installation bench space, 23 environment, 23 physical specifications, 24 power considerations, 22 power cords, 22 pump module, 35 interface board, 131 interface cable, 38 interfaces, 19
P
packaging shipping container, 30 packaging, damaged, 30 parts accessory kit, 147 active inlet valve, 146 bottle head assembly, 136 cover, 142, 147 damaged, 30 foam, 142
164
Index
hydraulic path with solvent selection valve, 138 hydraulic path without solvent selection valve, 140 leak handling, 142 missing, 30 outlet ball valve, 144 pump head assembly with seal wash, 142 purge valve, 145 sheet metal kit, 142 solvent cabinet, 136 performance specifications, 25 pH range, 25 physical specifications, 24 humidity, 24 line voltage and frequency, 24 operating altitude, 24 operation temperature, 24 power consumption, 24 safety standards, 24 weight and dimensions, 24 piston, 101, 110 power considerations, 22 consumption, 24 cord, 36 cords, 22 power cable, 31 power cord, 36 power switch, 37 pressure operating range, 25 pulsation, 25 pressure pulsation, 16, 79 pressure range, 74 pressure ripple, 89 pressure signal, analog, 36 pressure test, 82 results, 88 priming with a pump, 48 PTFE frit, 102, 115, 145 pulsation pressure, 16 pump elasticity calibration, 92 pump head assembly with seal wash, 142 pump module
installation, 35 pump seals, 52, 101, 107 alternative material, 74 for normal phase solvents, 74 pump stroke AUTO mode, 17 purge valve, 52, 102, 115, 145
R
radio interference, 158 Rapid Resolution LC System, 32 rear view, single stack, 34 rear view, twin stack, 36 reassembling the pump head, 113 recommended pH range, 25 remote cable, 36 remote connector, 18 remove damper and mixer, 75 removing the pump head, 104 repair procedures, 101 repairs cleaning the instrument, 96 definition of, 94 introduction, 94 using the ESD strap, 97 warnings and cautions, 94 replacing firmware, 133 restriction capillary, 92 results pressure test, 85, 88 ripple composition, 89 pressure, 89 RS-232C connector, 18
S
safety information standards, 24 SB-C18, 2.1x50mm,1.8um,600bar, 31 SB-C18, 4.6x50mm, 1.8um, 600bar, 31 screwdriver pozidriv #1, 104, 107, 110, 111, 113, 124 screwdriver, flat-head, 111 seal wash wash solvent, 73
when to use, 73 seal wear, 67 seal wear counter, 108 seals, 52, 101, 126 alternative material, 74 normal phase, 74 security lever, 37 setable flow range, 25 sheet metal kit, 142 shipping container, 30 sieve, 115, 121 signal analog, 36 detector, 36 pressure, analog, 36 simple repair procedures, 101 simple repairs exchanging active inlet valve cartridge, 115 exchanging AVI cartridge, 115 single stack front view, 33 rear view, 34 Site Requirements, 21 site requirements power considerations, 22 snap fastener, 41, 44 solubility, gas, 52 Solvent bottle transparent, 31 solvent bottles amber, 31, 70, 136 transparent, 136 solvent cabinet, 30, 42, 52, 136 solvent compressibility calibration, 89, 90 solvent filters algea, 70 checking, 70 cleaning, 71 prevent blockages, 70 solvent information, 54, 160 solvent inlet filter, 52, 136 solvent selection valve, 12, 30, 41, 124 solvent tubing, 136 solvents, 160 sonic bath, 121 sound emission, 159 specifications analog signal output, 26
165
Index
communications, 26 control and data evaluation, 26 performance, 25 physical, 24 stack configuration, 32 front view, single stack, 33 front view, twin stack, 35 rear view, single stack, 34 rear view, twin stack, 36 stroke volume, 16 Syringe, 30 adapter luer/barb, 30
operational hints, 72 when to use, 72 valve active inlet valve, 116 active inlet valve cartridge, 116 active inlet valve, replacement, 115 solvent selection, 124 variable stroke volume, 16 voltage range, 18 selector, 18
T
tests pressure test, 82 pressure test results, 85 pump elasticity calibration, 92 running the pressure test, 84 solvent compressibility calibration, 89, 90 tools blank nut, 1/16 inch, 84 hexagonal key 4 mm, 110, 111, 113 restriction capillary, 92 screwdriver pozidriv #1, 104, 107, 110, 111, 113, 124 wrench 1/4 - 5/16 inch, 84, 92 wrench 1/4 inch, 107 wrench 1/4 inch, slitted socket, 104 wrench 14 mm, 88, 90, 102, 116, 118, 121 tube screw, 136 tubing PTFE, 136 tweezers, 102 tools, 102 twin stack front view, 35 rear view, 36
W
wash seals, 101, 111 wash solvent, 73 weight and dimensions, 24 wrench 1/4 - 5/16 inch, 84, 92 wrench 1/4 inch, 107 wrench 1/4 inch, slitted socket, 104 wrench 14 mm, 88, 90, 102, 116, 118, 121
U
unpacking the pump, 30 User Manual, 31
V
vacuum degasser, 12, 27, 52
166
www.agilent.com
In This Book
This manual contains user information about the Agilent 1200 Series Binary Pump SL. The manual describes the following: introduction to the pump installation, optimizing performance, diagnostics and troubleshooting, maintenance and easy repairs, parts and materials, specifications.