Agilent SIPS 10, SIPS 20 User Guide

Agilent Sample Introduction Pump System SIPS 10/20
User’s Guide
Notices
© Agilent Technologies, Inc. 1995– 1997, 2003–2004, 2010, 2012
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.
Manual Part Number
8510132800
Edition
Eighth edition, March 2012
Agilent Technologies, Inc.
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.
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.
Restricted Rights Legend
If software is for use in the performance of a U.S. Government prime contract or subcontract, Software is delivered and licensed as “Commercial computer software” as defined in DFAR 252.227-7014 (June
1995), or as a “commercial item” as defined in FAR 2.101(a) or as “Restricted computer software” as defined in FAR 52.227-19 (June 1987) or any equivalent agency regulation or
contract clause. Use, duplication or disclosure of Software is subject to Agilent Technologies’ standard commercial license terms, and non­DOD Departments and Agencies of the U.S. Government will receive no greater than Restricted Rights as defined in FAR 52.227-19(c)(1-2) (June
1987). U.S. Government users will receive no greater than Limited Rights as defined in FAR 52.227-14 (June
1987) or DFAR 252.227-7015 (b)(2) (November 1995), as applicable in any technical data.
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.
WARNING
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.
2 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Contents
Contents
1. Safety Practices and Hazards 9
General 9
Hazard Warnings 10
Electrical Hazards 10
Moving Parts Hazard 10
Chemical Hazards 10
Other Precautions 11
Notes and Tips 11
Warning and Caution Messages 11
Warning Symbols 12
Information Symbols 13
Color Coding 13
CE Compliance 14
Electromagnetic compatibility 14
EN55011/CISPR11 14
ICES/NMB-001 15
2. Introduction 17
About this Manual 19
3. Specifications 21
Environmental 21
Power 22
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 3
Contents
External Connections 23
Weights and Dimensions 23
Weight 23
Dimensions (W × D × H) 23
Performance 24
4. Installation 25
Installation Checklist 26
Unpacking 26
Power 27
Checking the Fuses 27
Installing the Pump Unit and Electronic Control Module 28
Cabling 30
Connecting to the Agilent AA/Computer 30
Connecting to the SIPS Unit 30
Installing the Pump Bands 32
Installing the Diluent Tubing 33
Connecting the SIPS to the Nebulizer 33
Installing the SIPS Pump Tubing 33
Extending the Pump Tubing 35
Calibrating the SIPS Pressure Arm Force 35
Computer-controlled Instruments 35
Standalone Agilent 50/55 AA Instruments 37
Conditioning the SIPS Pump Tubing 38
Fitting the Dust Cover 38
4 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Contents
Connection to an Autosampler 38
Rinse Solution 39
Replacing the Pump Tubing 39
5. Operation 41
Operational Tips 42
Nebulizer Setup 43
Automatic Calibration from a Single Standard 44
SIPS 10 44
SIPS 20 45
Automatic Calibration and Dilution of Overrange Samples 46
SIPS 10 46
SIPS 20 47
Autorun with QC Spikes (SIPS 20) 48
Online Addition of Chemical Modifier or Internal Standard (SIPS 20) 50
Using the Autosamplers and the SIPS 10 51
Single Pump SIPS 20 Operation 52
Standard Additions Calibration 53
SIPS 20 53
SIPS 10 55
6. Command Reference 57
Method Window 58
Type/Mode Page 58
Measurement Page 58
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Contents
SIPS Page 58
Standards Page 62
QC Tests Page 63
Sequence Parameters Window 64
Options Page 64
Analysis Window 64
Calibrate Pumps 64
Determine SIPS LRR 65
Flame Facilities Dialog 65
Load 65
Unload 65
Purge RH Pump 66
Purge LH Pump 66
Stop Pumps 66
Flame Optimization 66
Start Pump 66
Stop Pump 66
7. Maintenance 67
Daily 67
Weekly 70
Monthly 70
8. Troubleshooting 73
Two Pumps Not Connected 74
SIPS 10 74
SIPS 20 74
6 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Contents
Pump Calibration Failed! Switch to Single Pump Operation 74
Dual Pump SIPS or Diluter Required to Prepare Standard Additions 75
Unable to Achieve Blank Reading 75
No Flame Detected – SIPS Operation Cannot Continue 76
Dilution Factor > 50 76
Dilution factor > 200 76
LRR Calibration Failed – Default LRR Value Used 77
SIPS Offline or Pump Not Connected 77
The SIPS Doesn't Pump 77
The Absorption Signal Drifts Over Time 78
Poor Sensitivity 78
Poor Precision 79
There are Spikes in the Absorbance Signal 79
The Accuracy of the Result is Poor 79
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 7
Contents
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8 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Safety Practices and Hazards
1. Safety Practices and Hazards
General 9
Hazard Warnings 10
Electrical Hazards 10
Moving Parts Hazard 10
Chemical Hazards 10
Other Precautions 11
Notes and Tips 11
Warning and Caution Messages 11
Warning Symbols 12
Information Symbols 13
Color Coding 13
CE Compliance 14
Electromagnetic compatibility 14
General
Operation of the Sample Introduction Pump System (SIPS) accessory involves the use of high voltage and moving parts. Careless, improper or unskilled use of this accessory can cause death or serious injury to personnel, or severe damage to equipment and property.
Appropriate safety practices have been included in this operation manual and your spectrometer operation manual to help you operate the equipment safely. Read all safety practices thoroughly before attempting to operate your system.
If the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired.
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 9
Safety Practices and Hazards
Hazard Warnings
In addition to the hazard warnings specified in your spectrometer operation manual, specific hazard warnings have been included in this operation manual. These warnings state the hazard, describe how to avoid it and specify the possible consequences of not following the instructions. Read all warnings carefully and observe them at all times.
Electrical Hazards
The SIPS electronic control module contains electrical circuits, devices and components operating at dangerous voltages. Contact with these circuits, devices and components can cause death, serious injury or painful electric shock. Panels or covers retained by screws on the SIPS may be opened only by an Agilent field service engineer.
A blown fuse should be replaced only with one of the size and rating specified in the text adjacent to the fuse holder. Always ensure that the accessory is turned off and disconnected from the mains supply before attempting any replacement.
Moving Parts Hazard
During normal operation of the SIPS accessory, there are rotating and automatic clamping components. To avoid injury or damage ensure that all fingers, clothing etc. are kept well clear of these parts during operation.
Chemical Hazards
The SIPS accessory may involve the use of materials that are corrosive or otherwise hazardous. Careless, improper or unskilled use of these materials can cause serious personal injury or an environmental hazard.
Always ensure that laboratory safety practices governing the use, handling and disposal of hazardous materials are strictly observed. These safety practices should include wearing the appropriate safety clothing.
10 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Safety Practices and Hazards
Always ensure that the sample introduction system is thoroughly flushed with distilled water and that the contents of the drain or waste container are known and disposed of if necessary before touching any part.
Other Precautions
The pump module of the SIPS accessory weighs approximately 5.5 kg (12 lb). To avoid injury or damage to the pump module, take care when lifting or moving the accessory so as not to drop it.
The use of the SIPS in any manner other than that specified by Agilent may impair the protection provided by the product.
Notes and Tips
A Note or Tip message is used to give advice or additional information
NOTE
This is a note.
Warning and Caution Messages
A Warning message is used in the text when failure to observe instructions or precautions could result in death or injury.
WARNING
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 11
Name of Warning Detail of hazard. Information on how to avoid the hazard.
Safety Practices and Hazards
A Caution message is used when failure to observe instructions could result in damage to equipment (Agilent supplied and/or other associated equipment).
CAUTION
Warning Symbols
This is a caution statement.
The following is a list of symbols that appear in conjunction with warnings in this manual and on the spectrometer. The hazard they describe is also shown.
A triangular symbol indicates a warning. The meanings of the symbols that may appear alongside warnings in the documentation or on the instrument itself are as follows:
Corrosive liquid
Hot surface
Electrical shock
Moving parts
Fire hazard
Noxious gas
Heavy weight
(danger to feet)
Heavy weight
(danger to hands)
The following symbol may be used on warning labels attached to the instrument. When you see this symbol, refer to the relevant operation or service manual for the correct procedure referred to by that warning label.
12 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Safety Practices and Hazards
Information Symbols
The following symbols appear on the instrument for your information.
I
0
Color Coding
The various indicator lights appearing on the instrument and any associated accessories have been color coded to represent the status of the instrument or accessory:
Mains power on
Mains power off
Fuse
Single phase alternating current
When attached to the rear of the instrument, indicates that the product complies with the requirements of one or more EU directives.
When attached to the rear of the product, indicates that the product has been certified (evaluated) to CSA 61010.1 and UL 61010-1.
A green light indicates the instrument is in normal standby condition.
A blue light indicates that operator intervention is required.
An orange light indicates a potential hazard.
A red light indicates danger or an emergency.
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 13
Safety Practices and Hazards
CE Compliance
Your SIPS has been designed to comply with the requirements of the Electro-magnetic Compatibility (EMC) Directive and the Low Voltage (electrical safety) Directive (commonly referred to as the LVD) of the European Union. Agilent has confirmed that each product complies with the relevant Directives by testing a prototype against the prescribed EN (European Norm) standards.
Proof that a product complies with the Directives is indicated by:
The CE Marking appearing on the rear of the product.
The documentation package that accompanies the product,
containing a copy of the Declaration of Conformity. This Declaration is the legal declaration by Agilent that the product complies with the Directives, and also shows the EN standards to which the product was tested, to demonstrate compliance.
Electromagnetic compatibility
EN55011/CISPR11
Group 1 ISM equipment: group 1 contains all ISM equipment in which there is intentionally generated and/or used conductively coupled radio- frequency energy which is necessary for the internal functioning of the equipment itself.
Class A equipment is equipment suitable for use in all establishments other than domestic and those directly connected to a low voltage power supply network which supplies buildings used for domestic purposes.
This device complies with the requirements of CISPR11, Group 1, Class A as radiation professional equipment. Therefore, there may be potential difficulties in ensuring electromagnetic compatibility in other environments, due to conducted as well as radiated disturbances.
14 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Safety Practices and Hazards
Operation is subject to the following two conditions:
1 This device may not cause harmful interference.
2 This device must accept any interference received, including
interference that may cause undesired operation.
If this equipment does cause harmful interference to radio or television reception, which can be determined by turning the equipment off and on, the user is encouraged to try one or more of the following measures:
1 Relocate the radio or antenna.
2 Move the device away from the radio or television.
3 Plug the device into a different electrical outlet, so that the device
and the radio or television are on separate electrical circuits.
4 Make sure that all peripheral devices are also certified.
5 Make sure that appropriate cables are used to connect the device
to peripheral equipment.
6 Consult your equipment dealer, Agilent Technologies, or an
experienced technician for assistance.
7 Changes or modifications not expressly approved by Agilent
Technologies could void the user’s authority to operate the equipment.
ICES/NMB-001
This ISM device complies with Canadian ICES- 001.
Cet appareil ISM est conforme à la norme NMB-001 du Canada.
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 15
Safety Practices and Hazards
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16 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Introduction
2. Introduction
About this Manual 19
The Sample Introduction Pump System (SIPS) is an integrated, efficient dilution system for flame AA and is suitable for use with most Agilent (flame) atomic absorption spectrometers.
In some instruments the control module is built in to the instrument (e.g., the Agilent 280FS AA). For these instruments, installation instructions for the control module can be ignored. It is still necessary to unpack and install the SIPS pump module.
The unique range of capabilities and applications provided by the SIPS includes:
Online 10 point calibration from a single standard
Online standard additions calibration from a single standard
Intelligent online dilution of overrange samples with ‘Smart
Rinse' to reduce memory effects
Online preparation of analytical spikes, using a single standard
Online addition of chemical modifiers such as ionization
suppressants, releasing agents or internal standards
An extended dynamic range for flame AA, approaching that of
ICP-OES
The SIPS accessory is available as a single pump (SIPS 10) or dual pump system (SIPS 20). The SIPS 10 provides online calibration and sample dilution, while the SIPS 20 provides the added capabilities possible with dual pump operations, including online standard additions calibration, spiking of samples and addition of modifiers.
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 17
Introduction
CAUTION
The SIPS is not suitable for use with organic solvents because the tubing is not resistant to these solvents.
to nebulizer
continuous flow
diluent
sample
Figure 1 The SIPS 10 single pump unit
The SIPS 10 uses a single pump to combine the sample (or a bulk standard) with a small flow of diluent. Reducing the pump speed results in a reduced flow of sample. With the nebulizer uptake rate constant, the diluent flow is increased, effectively diluting the sample. Using accurate computer control of the pump speed, online dilution and automatic calibration are possible.
18 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Introduction
to nebulizer
continuous
continuous
flow
flow
diluent
Figure 2 The SIPS 20 dual pump system
The SIPS 20 uses two pumps to deliver sample and a standard or modifier to the nebulizer. Controlling the relative speeds of both pumps in the SIPS 20 allows the amount of standard or modifier added to the sample to be precisely regulated, facilitating online standard additions calibration, spiking of samples and addition of modifiers. Samples can still be diluted online by reducing the sample pump speed relative to the speed of the second pump.
SIPS supports both manual and automatic sampling with the Agilent flame autosamplers. The diluter option for the Agilent SPS 3 autosampler is not required and cannot be used in conjunction with SIPS, since the SIPS automatically provides all dilution operations.
About this Manual
This manual includes instructions for installing, using and maintaining the SIPS. It is intended for use by laboratory personnel responsible for the day-to-day use of an Agilent AA instrument fitted with a SIPS unit.
sample
standard or modifier
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 19
Introduction
The manual does not include instructions for setting up and operating your spectrometer. For these instructions refer to the Agilent Atomic Absorption spectrometer (AA) operation manual supplied with your instrument.
20 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Specifications
3. Specifications
Environmental 21
Power 22
External Connections 23
Weights and Dimensions 23
Environmental
Your accessory is designed for indoor use only. In addition, this accessory is suitable for the following categories:
Installation category II
Performance 24
Pollution degree 2
Equipment class I
Condition Altitude Temp t (°C) Humidity (%RH)
non-condensing
Non-operating (transport) 0–2133 m (0-7000 ft) 5–45 20–80
Operating within performance specifications
0–853 m (0–2800 ft)
853–2133 m (2800–7000 ft)
10–35 10–25
8–80
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 21
Specifications
NOTE
Power
NOTE
For optimum analytical performance, it is recommended that the ambient temperature of the work area be between 20 and 25 °C (68 and 77 °F) and be held constant to within ±2 °C throughout the entire working day.
If you are using an Agilent 280FS AA or 140/240 AA1, the electronic module is built into the instrument. A separate power supply is not required. The electronic module is powered from the main spectrometer power supply.
Information is correct at time of printing — information on the back of the accessory is the most up to date.
Voltage
Frequency
Consumption
100–240 VAC ±10%
50-60 Hz ± 1 Hz
70 W
NOTE
For safety reasons, any other internal fuse or circuit breaker is not operator accessible, and should be replaced only by an Agilent field service engineer.
1
Factory fitted option
22 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Specifications
External Connections
Mains power cord connector:
Australia
10 A 250 VAC Complies with AS3112
USA
Europe
10 A 125 VAC Complies with NEMA 5-15P
6A 250 VAC Complies with CEE7 sheet vii or NFC61.303VA
Other connections:
IEEE-488
Pump module interconnection: 25-pin D-range connector
Mains inlet coupler: 6 A 250 VAC IEC type.
Weights and Dimensions
Weight
Packed
Unpacked
- pump module
- electronic control module
Dimensions (W × D × H)
15 kg (33 lb)
5.5 kg (12 lb)
2
3 kg (6.6 lb)
Packed
Unpacked
- pump module
- electronic control module
620 × 530 × 360 mm (21 × 24.4 × 14.2 in.)
275 × 285 × 215 mm (10.8 × 11.2 × 8.5 in.)
2
225 × 100 × 385 mm (8.9 × 4 × 15.2 in.)
2
The optional electronic module is built into the Agilent 280FS AA or 140/240 AA, as a factory fitted option.
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 23
Specifications
Performance
Typical dilution error is < 2%.
Guaranteed performance (based on 3 × 3 second replicate readings using Integration with 30 second read delay time and 10 samples) is:
Dilution Factor
< 50
Dilution Error
Precision (% RSD)
< 3.5%
< 2.5%
24 Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide
Installation
4. Installation
Installation Checklist 26
Unpacking 26
Power 27
Installing the Pump Unit and Electronic Control Module 28
Cabling 30
Installing the Pump Bands 32
Installing the Diluent Tubing 33
Connecting the SIPS to the Nebulizer 33
Installing the SIPS Pump Tubing 33
Extending the Pump Tubing 35
Calibrating the SIPS Pressure Arm Force 35
Conditioning the SIPS Pump Tubing 38
Fitting the Dust Cover 38
Connection to an Autosampler 38
Rinse Solution 39
Replacing the Pump Tubing 39
Those sections covering the installation of the electronic control module are not relevant when the control module is built into the instrument, such as in the Agilent 280FS AA. It will still be necessary to unpack and install the SIPS pump module.
Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 25
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