Agilent Technologies Quaternary Pump 1100 User Manual 2

Agilent 1100 Series

Quaternary Pump

Reference Manual

sa

Copyright Agilent

Technologies 1999

All rights reserved. Reproduction, adaption, or translation without prior written permission is prohibited, except as allowed under the copyright laws.

Part No. G1311-90003

Edition 01/00

Printed in Germany

Warranty

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.

WARNING

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.

4

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

3Troubleshooting and Test Functions

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

Status Indicators 45

5

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

6

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

4Repairing 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

7

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

5Parts 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

8

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

6Introduction to the Quaternary Pump

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

connectors 197

9

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

10

Contents

Radio Interference 264

Sound Emission 264 Solvent Information 265

Agilent Technologies on Internet 266

11

Contents

12

1

Installing the Pump

How to install the quaternary pump

WA R NI N G

WA R NI N G

WA R NI N G

WA R NI N G

Installing the Pump

Site Requirements

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.

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.

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.

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.

Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.

14

N O T E

CA U T IO N

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.

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.

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.

15

Installing the Pump

Site Requirements

Table 1	Physical Specifications
Type		Specification	Comments
Weight		11 kg (25 lbs)
Dimensions		140 × 345 × 435 mm
(height × weight × depth)		(5.5 × 13.5 × 17 inches)
Line voltage		100–120 or 220–240 VAC, ± 10%	Wide-ranging capability
Line frequency		50 or 60 Hz, ± 5%
Power consumption		220 VA	Maximum
Ambient operating temperature		4–55 °C (41–131 °F)
Ambient non-operating temperature		-40–70 °C (-4–158 °F)
Humidity		< 95%, at 25–40 °C (77–104 °F)	Non-condensing
Operating Altitude		Up to 2000 m (6500 ft)
Non-operating altitude		Up to 4600 m (14950 ft)	For storing the quaternary
			pump
Safety standards: IEC, CSA, UL		Installation Category II, Pollution Degree 2

16

CA U T IO N

Table 2

Installing the Pump

Unpacking the Quaternary 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.

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.

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	4	(G1322-67300)
degasser
Power cables	2

17

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

18

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

19

Installing the Pump

Optimizing the Stack Configuration

	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)

Solvent cabinet

Vacuum degasser

Quaternary pump

Autosampler

Flow connections in the stack:

Example setup with 0.17mm ID green capillaries

Solvent bottles - degasser:

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:

G1313-87305 (SST, green)

Column compartment - column:

	G1316-87300 (SST, green)
	Column - detector:
Column compartment
	DAD G1315-87311 (SST, coated)
	VWD 5062-8522 (PEEK)
	Detector - waste:

Detector

N O T E

DAD 0890-1713 (PTFE, wide bore) VWD 5062-8535 (PEEK)

5062-2463 (corrugated waste tubing, reorder pack)

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.

20

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
N O T E	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.

21

Installing the Pump

Installing the Quaternary 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

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

2Ensure the power switch on the front of the quaternary pump is OFF (switch stands out).

Figure 3

Front of Quaternary Pump

Status Lamp

Power Switch

Serial number

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

4Connect 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.

5Connect the required interface cables to the quaternary pump.

22

		Installing the Pump
		Installing the Quaternary Pump
N O T E		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 LANboard) 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

6Connect all capillaries, solvent tubes and waste tubing (see “Flow Connections of the Quaternary Pump” on page 25).

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

23

Installing the Pump

Installing the Quaternary Pump

N O T E	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.

8Purge the quarternary pump (see “Priming and Purging the System” on page 28).

WA R NI N G	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.
N O T E	The pump was shipped with default configuration settings. To change these
	settings, see “Setting the 8-bit Configuration Switch” on page 223.

24

Installing the Pump

Flow Connections of the Quaternary 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
WA R NI 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.
	1 Remove the front cover by pressing the snap fasteners on both sides.
Figure 5		Removing the Front Cover

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

3Put the bottle-head assemblies into solvent reservoirs containing your mobile phase and place the bottle in the solvent cabinet.

4Connect 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.

25

Installing the Pump

Flow Connections of the Quaternary Pump

5Connect the solvent tubes to the outlet connectors (typically right connection of the channel) of the vacuum degasser.

6Connect the syringe adapter from the degasser accessory kit to the solvent tube of channel A.

7Using a piece of sanding paper connect the waste tubing to the purge valve and place it into your waste system.

8If 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.

9Connect the pump outlet capillary (quaternary pump to injection device) to the outlet of the purge valve.

10Prime your system before first use (see “Priming and Purging the System” on page 28).

26

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)

27

Installing the Pump

Priming and Purging the System

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.
WA R NI 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.
	Priming with a Syringe
	Before using a new degasser or new tubings for the first time:

1Prime 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:

2Replace 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.

3Disconnect solvent outlet tube of the channel that is supposed to be primed from your pump.

4Connect syringe adapter to solvent outlet tube.

28

Installing the Pump

Priming and Purging the System

5Push syringe adapter onto syringe.

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

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

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

9Disconnect syringe adapter from solvent tube.

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

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

N O T E	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.

N O T E

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.

1Open the purge valve of your pump (by turning it counterclockwise) and set flow rate to 3-5 ml/min.

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

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

4Pump for approximately 10 minutes before starting your application.

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

29

Installing the Pump

Priming and Purging the System

Table 5	Choice of Priming Solvents for Different Purposes
	Activity	Solvent	Comments
	After an installation	Isopropanol	Best solvent to flush air out of
			the system
	When switching between	Isopropanol	Best solvent to flush air out of
	reverse phase and normal		the system
	phase (both times)
	After an installation	Ethanol or Methanol	Alternative to Isopropanol
			(second choice) if no
			Isopropanol is available
	To clean the system when	Bidistilled water	Best solvent to re-dissolve
	using buffers		buffer cristals
	After a solvent change	Bidistilled water	Best solvent to re-dissolve
			buffer cristals
	After the installation of	Hexane + 5% Isopropanol	Good wetting properties
	normal phase seals (P/N
	0905-1420)

30