Agilent Technologies Quaternary Pump 1100 User Manual 2

Agilent 1100 Series Quaternary Pump

Reference Manual

 Copyright Agilent

Technologies 1999

Part No. G1311-90003

Edition 01/00

Printed in Germany

Warra nty

The information contained in this document is subject to change without notice.

Agilent Technologies makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties or merchantability and fitness for a particular purpose.

Agilent Technologies shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material.

WAR N ING

For details of safety, see Safety Information on page 260.

Warning Symbols Used In This Book

The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect the apparatus against damage.

Agilent Technologies Hewlett-Packard-Strasse 8 76337 Waldbronn Germany

Agilent 1100 Series Quaternary Pump

Reference Manual

In This Book

This manual contains technical reference information about the Agilent 1100 Series quaternary pump. The manual describes the following:

• installation,

• optimizing performance,

• troubleshooting,

• repairing,

• parts and materials,

• theory of operation, and

• specifications.

Contents

1 Installing the Pump

How to install the quaternary pump 13

Site Requirements 14 Unpacking the Quaternary Pump 17 Optimizing the Stack Configuration 20 Installing the Quaternary Pump 22 Flow Connections of the Quaternary Pump 25 Priming and Purging the System 28

2 Optimizing Performance

How to optimize the quaternary pump to achieve best chromatographic results 31

Hints for Successful Use of the Quaternary Pump 32 Solvent Information 34 Prevent Blocking of Solvent Filters 35 Operational Hints for the Vacuum Degasser 36 Operational Hints for the Multi Channel Gradient Valve (MCGV) 37 When to use the Continuous Seal Wash Option 38 When to Use Alternative Seals 39 Optimize the Compressibility Compensation Setting 40

3 Troubleshooting and Test Functions

The quaternary pump’s built-in troubleshooting and test functions 43

Status Indicators 45

Contents

Power Supply Indicator 46 Pump Status Indicator 46

Error Messages 47

Timeout 48 Shut-Down 49 Remote Timeout 50 Synchronization Lost 51 Leak 52 Leak Sensor Open 53 Leak Sensor Short 54 Compensation Sensor Open 55 Compensation Sensor Short 56 Fan Failed 57 Open Cover 58 Restart Without Cover 59 Zero Solvent Counter 60 Pressure Above Upper Limit 61 Pressure Below Lower Limit 62 Pressure Signal Missing 63 Missing Pressure Reading 64 Pump Configuration 65 Valve Fuse 66 Inlet-Valve Fuse 67 Valve Failed 68 Motor-Drive Power 69 Encoder Missing 70 Inlet-Valve Missing 71 Temperature Out of Range 72 Temperature Limit Exceeded 73 Servo Restart Failed 74

Contents

Pump Head Missing 75 Index Limit 76 Index Adjustment 77 Index Missing 78 Stroke Length 79 Initialization Failed 80 Wait Timeout 81

Pressure Test 82

Running the Pressure Test 84 Evaluating the Results 86

Leak Test 88

Running the Leak Test 90 Evaluating the Results 92

4 Repairing the Pump

Instructions on simple, routine repair procedures as well as more extensive repairs requiring exchange of internal parts 97

Cleaning the Quaternary Pump 99 Using the ESD Strap 100 Overview 101

Simple Repair Procedures 102

Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve 103 Exchanging the Outlet Ball Valve 106 Exchanging the Purge Valve Frit or the Purge Valve 108

Contents

Removing and Disassembling the Pump Head Assembly 110 Exchanging the Pump Seals and Seal Wear-in Procedure 112 Exchanging the Plungers 115 Installing the Continuous Seal Wash Option 116 Exchanging the Wash Seals 119 Reassembling the Pump Head Assembly 121 Exchanging the Multi-Channel Gradient Valve (MCGV) 123 Exchanging the optional Interface Board 126

Exchanging Internal Parts 127

Removing the Top Cover and Foam 128 Exchanging the Low Pressure Pump Main Board (LPM Board) 131 Exchanging the Damper 138 Exchanging the Fan 141 Exchanging the Pump Drive 143 Exchanging the Power Supply 147 Exchanging the Leak Sensor 152 Exchanging the Status Light Pipe 154 Assembling the Main Cover 155 Replacing the Top Cover and Foam 156

5 Parts and Materials

Detailed illustrations and lists for identification of parts and materials 159

Overview of Main Assemblies 160

Control Module (B-version) 163 Solvent Cabinet 164

Contents

Bottle Head Assembly 165 Hydraulic Path 166 Cover Parts 167 Sheet Metal Kit 168 Foam Parts 169 Power and Status Light Pipes 170 Leak Parts 171 Pump Head Assembly 172 Pump Head Assembly with Seal Wash Option 174 Outlet Ball Valve Assembly 176 Purge Valve Assembly 177 Active Inlet Valve Assembly 178 Accessory Kit G1311-68705 179 Seal Wash Option Kit 01018-68722 180

Cable Overview 181

Analog Cables 183 Remote Cables 185 BCD Cables 190 Auxiliary Cable 192 CAN Cable 192 External Contact Cable 193 RS-232 Cable Kit 194 LAN Cables 195

6 Introduction to the Quaternary Pump

An introduction to the pump, instrument overview, theory of operation, external communication and internal connectors 197

Contents

Introduction to the Quaternary Pump 198 Overview 199 Electrical Connections 204 Instrument Layout 206 Early Maintenance Feedback (EMF) 207 The Electronics 209 The Low-Pressure Pump Main Board (LPM) 210 Firmware Description 214 Optional Interface Boards 216 Agilent 1100 Series Interfaces 218 Setting the 8-bit Configuration Switch 223 The Main Power Supply Assembly 228

7 Control Module Screens for the Quaternary Pump

Screens available from the Analysis screen 233 Screens available from the System screen 242 Screens available from the Records screen 244 Diagnostics and Tests 251

8 Specifications

Performance specifications of the quaternary pump 253

Performance Specifications 254

Warranty Statement 257 Safety Information 260 Lithium Batteries Information 263

Contents

Radio Interference 264 Sound Emission 264 Solvent Information 265 Agilent Technologies on Internet 266

Contents

1 Installing the Pump

How to install the quaternary pump

Installing the Pump

Site Requirements

A suitable environment is important to ensure optimum performance of the quaternary pump.

Power Consideration

The quaternary pump power supply has wideranging capability (see Table 1 on page 16). It accepts any line voltage in the range described in the above mentioned table. Consequently there is no voltage selector in the rear of the quaternary pump. There are also no externally accessible fuses, because automatic electronic fuses are implemented in the power supply.

WARNING To disconnect the quaternary 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.

WARNING Shock hazard or damage of your instrumentation can result, if the

devices are connected to a line voltage higher than specified.

Power Cords

Different power cords are offered as options with the quaternary pump. The female end of each of the power cords is identical. It plugs into the power-input socket at the rear of the quaternary pump. The male end of each of the power cords is different and designed to match the wall socket of a particular country or region.

WARNING Never operate your instrumentation from a power outlet that has no

ground connection. Never use a power cord other than the power cord designed for your region.

WARNING Never use cables other than the ones supplied by Agilent Technologies

to ensure proper functionality and compliance with safety or EMC regulations.

Installing the Pump

Site Requirements

Bench Space

The quaternary pump dimensions and weight (see Table 1 on page 16) allow to place the quaternary pump on almost any laboratory bench. It needs an additional 2.5 cm (1.0 inches) of space on either side and approximately 8 cm (3.1 inches) in the rear for the circulation of air and electric connections.

If the bench should carry a complete Agilent 1100 Series system, make sure that the bench is designed to carry the weight of all the modules.

NOTE The pump should be operated in a horizontal position!

Environment

Your quaternary pump will work within specifications at ambient temperatures and relative humidity as described in Table 1 on page 16.

CAUTION Do not store, ship or use your quaternary pump under conditions where

temperature fluctuations could cause condensation within the quaternary pump. Condensation will damage the system electronics. If your quaternary pump was shipped in cold weather, leave it in its box and allow it to warm slowly to room temperature to avoid condensation.

Installing the Pump

Site Requirements

Table 1 Physical Specifications

Type Specification Comments

Weight 11 kg (25 lbs)

Dimensions (height × weight × depth)

Line voltage

Line frequency

Power consumption 220 VA Maximum

Ambient operating temperature

Ambient non-operating temperature

Humidity

Operating Altitude Up to 2000 m (6500 ft)

Non-operating altitude Up to 4600 m (14950 ft) For storing the quaternary

Safety standards: IEC, CSA, UL Installation Category II, Pollution Degree 2

140 × 345 × 435 mm (5.5 × 13.5 × 17 inches)

100–120 or 220–240 VAC,

50 or 60 Hz,

4–55

-40–70

< 95%, at 25–40

± 5%

°C (41–131 °F)

°C (-4–158 °F)

°C (77–104 °F)

± 10%

Wide-ranging capability

Non-condensing

pump

Installing the Pump

Unpacking the Quaternary Pump

Damaged Packaging

Upon receipt of your quaternary pump, inspect the shipping containers 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 quaternary 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 the carrier’s inspection.

CAUTION If there are signs of damage to the quaternary pump, please do not attempt to

install the quaternary pump.

Delivery Checklist

Ensure all parts and materials have been delivered with the quaternary pump. The delivery checklist is shown in Table 2. To aid in parts identification, please see Chapter 5 “Parts and Materials”. Please report missing or damaged parts to your local Agilent Technologies sales and service office.

Table 2 Quaternary Pump Checklist

Description Quantity

Quaternary pump 1

Solvent cabinet 1 (5062-8581)

Solvent bottles 4 (3 transparent 9301-1420, 1 amber 9301-1450)

Bottle head assembly 4 (G1311-60003)

Waste tube, purge valve 1 (5042-2461, reorder number, 5m)

Vacuum degasser 1

Solvent tubes for the degasser

Power cables 2

4 (G1322-67300)

Installing the Pump

Unpacking the Quaternary Pump

Table 2 Quaternary Pump Checklist, continued

Description Quantity

CAN cable 1

Remote cable As ordered

Signal cable As ordered

Reference Manual 2 (1 for the pump, 1 for the degasser)

Accessory kit (see Table 3) 1

Accessory Kit Contents — Quaternary Pump

Table 3 Accessory Kit Contents G1311-68705

Description Part Number Quantity

Capillary, pump to injection device G1312-67305 1

Seal insert tool 01018-23702 1

Wrench; 1/4 – 5/16 inch 8710-0510 1

Wrench; 14 mm 8710-1924 1

ESD wrist strap

9300-1408 1

Hex key 4mm 8710-2392 1

Waste tube (reorder number, 5m) 5062-2463 1.2 m

Velocity regulator (reorder number) 5062-2486 2

PTFE Frit 01018-22707 5

ESD: Electrostatic Discharge

Installing the Pump

Unpacking the Quaternary Pump

Accessory Kit Contents—Vacuum Degasser

Table 4 Accessory Kit Contents G1322-68705

Description Part Number Quantity

Syringe 5062-8534 1

Syringe adapter 9301-1337 1

Waste tube (reorder number, 5m) 5062-2463 1.2 m

Connecting tubes labeled A to D G1322-67300 4

Installing the Pump

Optimizing the Stack Configuration

If your quaternary pump is part of a complete 1100 Series system, you can ensure optimum performance by limiting the configuration of the system stack to the following configuration. This configuration optimizes the system flow path, ensuring minimum delay volume.

Figure 1 Recommended Stack Configuration (Front View)

Flow connections in the stack: Example setup with 0.17mm ID green capillaries

Solvent bottles - degasser:

Solvent cabinet

Vacuum degasser

Quaternary pump

G1311-60003 (bottle-head assembly, PTFE-tubings)

Degasser - pump:

G1322-67300 (PTFE-tubings)

Pump - autosampler:

G1312-67305 (SST, green)

Pump purge valve - waste:

5062-2461 (PTFE tubing wide bore, reorder pack)

Control Module

Autosampler

Column compartment

Detector

Autosampler - column compartment:

G1313-87305 (SST, green)

Column compartment - column:

G1316-87300 (SST, green)

Column - detector:

DAD G1315-87311 (SST, coated) VWD 5062-8522 (PEEK)

Detector - waste:

DAD 0890-1713 (PTFE, wide bore) VWD 5062-8535 (PEEK) 5062-2463 (corrugated waste tubing, reorder pack)

NOTE For a detailed view of the flow connections refer to the section “Flow

Connections” in chapter 1 of the reference manuals of the individual modules.

Installing the Pump

Optimizing the Stack Configuration

Figure 2 Recommended Stack Configuration (Rear View)

Remote cable 5061-3378

Pressure output to recorder, for PN see page 181

CAN Bus cable to handheld controller G1323-81600

CAN Bus cable for inter module communication 5181-1516 (0.5m) 5161-1519 (1.0m)

AC power

Analog signal to recorder,for PN see page 181

GPIB or LAN to ChemStation for PN see page 181

NOTE If a single stack configuration becomes too high, e.g. if an additional module

like a G1327A ALS Thermostat is added or if your bench is to high, a two stack configuration may be a better setup. Separate the stack between pump and autosampler and place the stack containing the pump on the right side of the stack containing the autosampler.

Installing the Pump

Installing the Quaternary Pump

Preparations Locate bench space.

Provide power connections. Unpack the pump.

Parts required Pump

Power cord, for other cables see text below and “Cable Overview” on page 181 ChemStation and/or Control Module G1323A/B

1 Place the quaternary pump on the bench in a horizontal position.

2 Ensure the power switch on the front of the quaternary pump is OFF (switch

stands out).

Figure 3 Front of Quaternary Pump

tatus Lamp

Power Switch

Serial number

3 At the rear of the quaternary pump move the security lever to its maximum

right position.

4 Connect the power cable to the power connector at the rear of the quaternary

pump. The security lever will prevent that the cover is opened while the power cord is connected to the quaternary pump.

5 Connect the required interface cables to the quaternary pump.

Installing the Pump

Installing the Quaternary Pump

NOTE In an Agilent 1100 Series system, the individual modules are connected

through CAN cables. The Agilent 1100 Series vacuum degasser is an exception . The vacuum degasser can be connected via the APG remote connector to the other modules of the stack. The AUX output allows the user to monitor the vacuum level in the degasser chamber. An Agilent 1100 Series control module can be connected to the CAN bus at any of the modules in the system except for the degasser. The Agilent ChemStation can be connected to the system through one GPIB or LAN (requires the installation of a LAN- board) cable at any of the modules (except for the degasser), preferably at the detector (MUST for the DAD). For more information about connecting the control module or Agilent ChemStation refer to the respective user manual. For connecting the Agilent 1100 Series equipment to non-Agilent 1100 Series equipment, see Chapter 6 “Introduction to the Quaternary Pump”

Figure 4 Rear of Quaternary Pump

Security lever

Slot for interface board

Analog pressure, 2mV/bar

APG Remote

RS-232C

CAN

GPIB Power

Configuration switch

6 Connect all capillaries, solvent tubes and waste tubing (see “Flow

Connections of the Quaternary Pump” on page 25).

7 Press in the power switch to turn on the quaternary pump.

Installing the Pump

Installing the Quaternary Pump

NOTE The power switch stays pressed in and a green indicator lamp in the power

switch is on when the quaternary pump is turned on. When the line power switch stands out and the green light is off, the quaternary pump is turned off.

8 Purge the quarternary pump (see “Priming and Purging the System” on page

28).

WARNING To disconnect the quaternary 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.

NOTE The pump was shipped with default configuration settings. To change these

settings, see “Setting the 8-bit Configuration Switch” on page 223.

Installing the Pump

Flow Connections of the Quaternary Pump

Preparations Pump is installed in the LC system.

Parts required Other modules

Parts from accessory kit, see “Accessory Kit Contents — Quaternary Pump” on page 18 Two wrenches 1/4–5/16 inch for capillary connections

WARNING 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.

1 Remove the front cover by pressing the snap fasteners on both sides.

Figure 5 Removing the Front Cover

2 Place the vacuum degasser and the solvent cabinet on top of the quaternary

pump.

3 Put the bottle-head assemblies into solvent reservoirs containing your mobile

phase and place the bottle in the solvent cabinet.

4 Connect the inlet tubes from the bottle-head assemblies to the inlet

connectors A to D (typically the left connection of the channel) of the vacuum degasser. Fix the tubes in the tube clips of the vacuum degasser.

Installing the Pump

Flow Connections of the Quaternary Pump

5 Connect the solvent tubes to the outlet connectors (typically right connection

of the channel) of the vacuum degasser.

6 Connect the syringe adapter from the degasser accessory kit to the solvent

tube of channel A.

7 Using a piece of sanding paper connect the waste tubing to the purge valve

and place it into your waste system.

8 If the quaternary pump is not part of a Agilent1100 System stack or placed on

the bottom of a stack, connect the corrugated waste tube to the waste outlet of the pump leak handling system.

9 Connect the pump outlet capillary (quaternary pump to injection device) to

the outlet of the purge valve.

10 Prime your system before first use (see “Priming and Purging the System” on

page 28).

Installing the Pump

Flow Connections of the Quaternary Pump

Figure 6 Flow Connections of the Quaternary Pump

Bottle-head assembly (G1311-60003)

Solvent cabinet

Vacuum degasser

Inlet

Outlet

Tube clip (1400-1578)

Tubings (G1322-67300)

Purge valve

Waste tubing (5062-2461)

Outlet capillary to autosampler (G1312-67305)

MCGV

Fitting for corrugated waste tubing (5062-2463, reorder pack, 5m)

Installing the Pump

Priming and Purging the System

The system can be primed either by drawing solvent through the degasser with a syringe or by pumping with the pump.

Priming the system with a syringe is recommended, when:

• vacuum degasser or connected tubings are used for the first time or vacuum tubes are empty or

• changing to solvents that are immiscible with the solvent currently in the vacuum tubes.

Priming the system by using the pump at high flow rate (3–5 ml/min) is recommended, when:

• pumping system was turned off for a length of time (for example, overnight) and if volatile solvent mixtures are used, or

• solvents have been changed.

WARNING When opening capillary or tube fittings solvents may leak out. Please

Priming with a Syringe

Before using a new degasser or new tubings for the first time:

1 Prime all tubings with at least 30 ml of iso-propanol no matter whether the

channels will be used with organic mobile phase or with water.

If you are changing to a solvent that is immiscible with the solvent currently in the tubing continue as follows:

2 Replace the current solvent with adequate organic solvent (see Table 5 on

page 30), if current solvent is organic or with water, if current solvent is an inorganic buffer or contains salt.

3 Disconnect solvent outlet tube of the channel that is supposed to be primed

from your pump.

4 Connect syringe adapter to solvent outlet tube.

Installing the Pump

Priming and Purging the System

5 Push syringe adapter onto syringe.

6 Pull syringe plunger to draw at least 30 ml of solvent through degasser and

tubing.

7 Replace the priming solvent with the new solvent of your choice.

8 Pull syringe plunger to draw at least 30 ml of solvent through degasser and

tubing.

9 Disconnect syringe adapter from solvent tube.

10 Connect the solvent tube to the appropriate channel of the MCGV.

11 Repeat step 3 to step 10 for the other solvent channels.

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 with your selected flow rate before starting any application. This will allow the vacuum degasser to properly degas the solvent in the degasser tubes.

NOTE The pump should never be used for priming empty tubings (never let the pump

run dry). Use the syringe to draw enough solvent for completely filling the tubings to the pump inlet before continueing to prime with the pump.

Priming with the Pump

When the pumping system has been turned off for a certain time (for example, overnight) oxygen will rediffuse into the solvent channels 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. Therefore priming of the vacuum degasser and the pumping system is required before starting an application.

1 Open the purge valve of your pump (by turning it counterclockwise) and set

flow rate to 3-5 ml/min.

2 Flush the vacuum degasser and all tubes with at least 30 ml of solvent.

3 Set flow to required value of your application and close the purge valve.

4 Pump for approximately 10 minutes before starting your application.

5 Repeat step 1 to step 4 for other solvent channels, where needed.

Installing the Pump

Priming and Purging the System

Table 5 Choice of Priming Solvents for Different Purposes

Activity Solvent Comments

After an installation

When switching between reverse phase and normal phase (both times)

After an installation Ethanol or Methanol Alternative to Isopropanol

To clean the system when using buffers

After a solvent change

After the installation of normal phase seals (P/N 0905-1420)

Isopropanol

Bidistilled water

Hexane + 5% Isopropanol Good wetting properties

Best solvent to flush air out of the system

(second choice) if no Isopropanol is available

Best solvent to re-dissolve buffer cristals

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