Agilent 7500 Series ICP-MS Hardware Manual Agilent Technologies
Notices © Agilent Technologies, Inc. 2008 Warranty 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. The material contained in this document is provided "as is," and is subject to being changed, without notice, in future editions.
Contents Figures Tables Preface F-1 T-1 P-1 Who Should Read This Book P-2 How to Use This Book P-2 Conventions Used in This Book P-3 Where to Go for More Information P-6 Agilent Technologies on the Internet P-6 Other Information P-6 1 Overview 1-1 Instrument Components 1-2 Agilent 7500 – Part Names 1-4 Front View 1-4 Rear View 1-6 Side View 1-8 Name of Gas Piping and Cooling Water Tubing Function of Components 1-12 Sample Introduction 1-14 ICP Source 1-15 Interface/Vacuum System 1-16 Ion Lenses 1-16 Oc
Contents RF Generator 1-20 Support Systems 1-21 Optional Equipment 1-21 Peripheral Equipment 1-22 Autosampler (I-AS) 1-22 ASX-500 Series Autosampler 1-22 EXR-8 Autosampler 1-22 Integrated Sample Introduction System (ISIS) Laser Ablation System 1-23 Plasma Chromatographic Software 1-23 Intelligent Sequence Software 1-23 Specifications 1-24 2 Precautions 1-22 2-1 Protective Earth 2-4 Closing the Instrument Panels and Hoods 2-4 Wearing Safety Glasses 2-4 Checking the Exhaust System 2-5 Handling Solvents C
Contents Product and environmental safety - toxic materials 2-12 Moving the Agilent 7500 ICP-MS 2-13 Environmental Conditions and Utility Requirements 2-13 Temperature and Humidity Ranges 2-13 Electromagnetic Compatibility 2-14 ICES/NMB-001 2-15 Electrical Power (Voltage, Frequency, Amperage, Phase) 2-15 Argon Gas Supply 2-15 Reaction Gas Supply (Agilent 7500cs, 7500cx) 2-15 Cooling Water 2-15 Exhaust Duct 2-15 Symbols Used on the Instrument 2-16 Others 2-17 Part Numbers 2-17 Serial Number 2-17 3 Startup,
Contents Scheduling Maintenance 4-3 Checking Lab Conditions 4-5 Maintenance Clocks 4-5 Viewing the Maintenance Clocks 4-6 Changing the Item Name 4-7 Setting the Maintenance Period 4-8 Resetting the Maintenance Clocks 4-8 Maintenance Log 4-9 Maintenance LogBook 4-9 Recording the Maintenance Log 4-11 The Maintenance Log Display 4-12 Deleting the Maintenance Log 4-13 Fuse 4-14 Cleaning the Frame 4-14 Sample Introduction 4-14 Peristaltic Pump Tubing 4-15 Cleaning the Peristaltic Pump Tubing 4-15 Replacing the
Contents Replacing or Refitting the Concentric Nebulizer and the End Cap 4-43 Cleaning the PFA Concentric Nebulizer 4-44 Removing the PFA Concentric Nebulizer 4-46 Installing the PFA Concentric Nebulizer 4-46 Cleaning the Spray Chamber and the Transfer Line 4-47 Cleaning the End Cap 4-48 Replacing or Refitting the Nebulizer and Spray Chamber 4-49 Testing the Nebulizer and Spray Chamber 4-50 Maintaining the Torch 4-51 Locating Tools and Supplies 4-51 Removing and Checking the Torch 4-52 Cleaning the Torch 4
Contents Locating Tools and Supplies 4-76 Working Inside the Vacuum Chamber 4-77 Removing the Extraction Lenses 4-80 Removing the Einzel Lens - Omega Lens Assembly 4-82 Removing Plate Bias Lens 4-85 Cleaning the Lenses 4-86 Refitting the Plate Bias Lens 4-88 Refitting the Einzel Lens - Omega Lens Assembly 4-88 Refitting the Extraction Lenses 4-90 Testing the Lenses 4-91 Maintaining the Lenses (Agilent 7500cs or 7500cx) 4-91 Locating Tools and Supplies 4-93 Working Inside the Vacuum Chamber 4-94 Removing th
Contents Dead Time Calibration 4-136 Troubleshooting 4-142 Maintaining the Penning Gauge 4-143 Locating Tools and Supplies 4-143 Removing the Penning Gauge 4-144 Refitting the Penning Gauge 4-145 Cleaning the Penning Gauge 4-146 Maintaining the Rotary Pumps 4-148 Locating Tools and Supplies 4-149 Changing the Rotary Pump Oil 4-149 Changing the Oil Mist Filter and Odor Element Testing the Rotary Pump 4-151 Maintaining the Water Strainer 4-152 Locating Tools and Supplies 4-152 Cleaning the Water Strainer 4-1
Contents PFA Concentric Nebulizer 6-7 Crossflow Nebulizer (CF) 6-7 Nebulizer Endcap 6-8 Spray Chamber 6-8 Quartz (QZ) 6-8 Polypropylene (PP) 6-8 Teflon (PFA) 6-9 [Reference] Pyrex Glass (PG) 6-9 ICP Torch 6-9 Interface 6-10 Ion Lenses - Principles of Operation 6-11 Extraction Lens 6-14 Einzel Lens 6-15 Omega Lens 6-15 Octopole Reaction System 6-17 Gas Flow Tuning 6-19 Q-pole 6-19 Electron Multiplier (EM) 6-21 APG remote interface 6-23 Appendix A-1 Appendix A.
Figures Figures Figure 1. Figure 2. Figure 3. Figure 4. Figure 5. Figure 6. Figure 7. Figure 8. Figure 9. Agilent 7500 (Front View) 1-4 Agilent 7500 (Rear View) 1-6 Agilent 7500 Side View (Left) 1-8 Name of Gas Piping and Cooling Water Tubing 1-9 Name of Gas Piping and Cooling Water Tubing 1-10 Water and Gas Flow Diagram 1-11 System Diagram (7500a) 1-13 Octopole Reaction System (7500cs/cx) 1-13 Nebulizer and Spray Chamber (Top: Babington type, Bottom: concentric type) 1-14 Figure 10.
Figures Figure 26. Running Time Dialog Box (Picture may differ depending on ICP-MS Model/Mode) 4-6 Figure 27. The Example of the Message 4-7 Figure 28. Maintenance LogBook window 4-9 Figure 29. The displayed item area of the Maintenance LogBook window 4-10 Figure 30. Change List Item Dialog Box. 4-10 Figure 31. Logbook Editor dialog box 4-11 Figure 32. Logbook Viewer Dialog Box 4-12 Figure 33. 4-13 Figure 34. Peristaltic Pump 4-16 Figure 35. Sample Introduction Maintenance dialog box 4-17 Figure 36.
Figures Figure 55. PFA Concentric Nebulizer 4-44 Figure 56. Nebulizer Orientation 4-47 Figure 57. End Cap Orientation (example: Babington Nebulizer) 4-49 Figure 58. ICP Torch 4-53 Figure 59. ICP Torch 4-54 Figure 60. Position of Torch Inside Work Coil 4-56 Figure 61. 4-58 Figure 62. Torch, Shield Plate and Bonnet 4-61 Figure 63. Torch, Shield Plate and Bonnet 4-63 Figure 64. Position of Torch Inside Work Coil 4-64 Figure 65. Shield Plate installation 4-65 Figure 66.
Figures Figure 82. Figure 83. Figure 84. Figure 85. Figure 86. Figure 87. Figure 88. Figure 89. Reaction Cell Assembly 4-102 Reaction Cell as Refitted 4-103 Plate Bias Wire 4-104 Reaction Cell Assembly Dismantled 4-105 Removing the Cell Entrance Lens 4-106 Securing the Octopole Plate 4-107 Removing the Cell Exit Lens 4-107 The Octopole with the Cell Entrance Lens and Cell Exit Lens Removed 4-108 Figure 90. Plate Bias Lens Location (with the Reaction Cell Assembly Removed) 4-109 Figure 91.
Figures Figure 108. EM and Vacuum Chamber 4-132 Figure 109. Hardware Settings dialog box 4-134 Figure 110. Change Detector Type dialog box 4-134 Figure 111. ICP-MS Configuration Window 4-136 Figure 112. Select Use Dead Time Calibration. 4-137 Figure 113. 4-138 Figure 114. Select Element for EM Dead time Calibration dialog box 4-138 Figure 115. 4-139 Figure 116. 50ppb check. 4-139 Figure 117. 50ppb finished. 4-140 Figure 118. 4-140 Figure 119. 1ppm Check. 4-141 Figure 120.
Figures Figure 137. APG Remote Connector Figure 138.
Tables Tables Table 1. P-4 Table 2. 1-24 Table 3. Meter Control Panel Values 3-16 Table 4. 3-18 Table 5. 3-18 Table 6. 3-18 Table 7. 3-19 Table 8. 3-19 Table 9. Maintenance Schedule 4-3 Table 10. Agilent 7500 Ion Lenses 4-91 Table 11. Remote Signals 6-23 Table 12.
Tables T-2 Agilent 7500 Series ICP-MS Hardware Manual
Agilent 7500 Series ICP-MS Hardware Manual Preface Who Should Read This Book P-2 How to Use This Book P-2 Conventions Used in This Book P-3 Where to Go for More Information P-6 Agilent Technologies on the Internet P-6 Other Information P-6 The Agilent 7500 Series ICP- MS Hardware Manual provides an instrument overview, safety precautions and procedures for optimization, maintenance and troubleshooting. Please read the chapters regarding the overview and safety information before using the instrument.
Preface Who Should Read This Book The primary audience for the Agilent 7500 Series ICP- MS Hardware Manual consists of chemists and instrument operators in a laboratory. To use this manual effectively, you should have a strong knowledge of chemistry, and at least a basic level of computer experience. How to Use This Book The Agilent 7500 Series ICP- MS Hardware Manual contains six chapters that can be accessed independently, as needed.
Preface Conventions Used in This Book This book uses certain conventions to distinguish different types of information easily. This section describes these conventions. Instructions All step- by- step instructions are numbered and in bold, as in the following example. 1 Select Instrument >> Tune from the ICP- MS Top. The Sensitivity tuning window appears.
Preface Terminology This book frequently uses the following terms: Table 1 P-4 Convention Information Press To hold down a button on the keyboard. Click To press and release the mouse button. Double-click To click the mouse button twice in rapid succession. Drag To press and hold the mouse button while moving the pointer. Active Window The window in which the cursor is currently located. Radio Buttons Choices where you can select only one item from a list.
Preface Notes Notes contain a reminder about the effect of particular actions. They are indicated as follows: NOTE This example shows how a note is displayed. Cautions Cautions indicate situations that could overwrite data or require immediate attention to prevent harm to the instrument. Cautions are indicated as follows: CAUTION This example shows how a caution is displayed. Warnings Warnings indicate situations that could cause bodily harm.
Preface Where to Go for More Information In addition to the Agilent 7500 Series ICP- MS Hardware Manual, you can reference the following resources: • Agilent 7500 Series ICP- MS MassHunter Workstation (G7200A) Operator’s Manual or Agilent 7500 Series ICP- MS ChemStation (G1834B) Operator’s Manual • Agilent 7500 Series ICP- MS Tuning and Application Handbook • Agilent 7500 Series ICP- MS Customer Maintenance Parts List • Agilent 7500 Series ICP- MS Site Preparation Guide • Online Help Agilent Technologie
Agilent 7500 Series ICP-MS Hardware Manual 1 Overview Instrument Components 1-2 Agilent 7500 – Part Names 1-4 Function of Components 1-12 Support Systems 1-21 Optional Equipment 1-21 Peripheral Equipment 1-22 Specifications 1-24 The Agilent Technologies 7500 Series ICP- MS (Agilent 7500) is an inductively coupled plasma mass spectrometer (ICP- MS). It can measure trace elements as low as one part per trillion (ppt) or quickly scan more than 70 elements to determine the composition of an unknown sample.
1 Overview Instrument Components This section describes the instrument components, starting with a general overview of the operating principles of the Agilent 7500. The general system consists of the following instruments. The auto sampler and the water chiller are optional. 1-2 1 ICP- MS Instrument Agilent 7500 ICP- MS 2 MassHunter Workstation (or ChemStation) MassHunter Workstation (or ChemStation) controls the Agilent 7500 ICP- MS, acquires data, and analyzes the acquired data.
Overview 1 The following steps provide a brief overview of how the Agilent 7500 analyzes a sample. More detail is provided in later sections. 1 The sample solution is pumped into the inlet system where it is nebulized, forming a fine sample aerosol. 2 The aerosol is then carried into a high temperature argon plasma which atomizes and ionizes the sample to produce a cloud of positively charged ions.
1 Overview Agilent 7500 – Part Names The names of the parts of the Agilent 7500 are described in this section. Front View Exhaust Duct Hood (left) Protective Tinted Window Hood (right) Plasma Off Switch (Shutdown Switch on the reverse side) LED Drain Tray Drain Tray Port Power Switch Peristaltic Pump Figure 1 1-4 Agilent 7500 (Front View) Hood (Left) This hood is used to cover the torch and interface area during operation.
Overview 1 Power Switch Main power switch of Agilent 7500. Before turning on this switch, you need to turn on the power breaker located on the rear side. When the power is on, the green indicator in the center of the switch lights green. NOTE WA R N I N G Plasma Off Switch When you push this switch for more than 1 second, the plasma will turn off and the instrument will transfer to standby mode. This switch is used to immediately shut off the plasma if an abnormal condition exists.
1 Overview Rear View Connection for the Rotary Pump(s) Exhaust Hose(s) Helium Gas Inlet Hydrogen Gas Inlet Argon Gas Inlet Optional Gas Inlet SERIAL A SERIAL B ETHERNET REMOTE Water Outlet Cooling Water Inlet Vacuum Hose Connection for the Rotary Pump Power Switch for the Rotary Pumps Main Power Breaker SERIAL A SERIAL B Ethernet or GPIB Interface Remote Port ETHERNET REMOTE Main Power Supply Cable Figure 2 1-6 Power Connection for the Rotary Pumps Agilent 7500 (Rear View) Agilent 7500
Overview Cooling Water Inlet/Outlet Cooling water inlet and outlet port Argon Gas Inlet Argon gas inlet port Optional Gas Inlet Optional gas inlet port Helium Gas Inlet Helium gas inlet port for Agilent 7500cs, 7500cx Hydrogen Gas Inlet Hydrogen gas inlet port for Agilent 7500cs. Optional for 7500cx. Main Power Supply Cable Power cable Main Power Breaker The main power supply circuit breaker.
1 Overview Side View Main Power Supply Cable Hold down holes for attaching to table Figure 3 Agilent 7500 Side View (Left) Hold down holes for attaching to a Table or bench. If you need to attach the Agilent 7500 to a table or bench, slots are provided as fastening points.
Overview 1 Name of Gas Piping and Cooling Water Tubing Figure 4 Name of Gas Piping and Cooling Water Tubing Agilent 7500 Series ICP-MS Hardware Manual 1-9
1 Overview Figure 5 1-10 Name of Gas Piping and Cooling Water Tubing Agilent 7500 Series ICP-MS Hardware Manual
Overview 1 Exhaust Duct Nebulizer SAMPLE INTRODUCTION AREA Peristaltic Spray Chamber TORCH BOX AREA Pump Filter ICP Sample Inlet Work Coil Peristaltic Pump Gate Valve Drain Vessel P Option Gas Solenoid Valve P Interface Chamber BP BP DP DP Filter Argon PSV Gas Solenoid Valve P T Evacuation Assist Valve (on 7500cx with H2 upgrade) I/F Solenoid Valve BP BP Backing & I/F Pirani Sensor PSV PSV Orifice Cooling Water Outlet Cooling Water Inlet VAC VALVE ASSY Rotary Pump Exhaust Inlet W
1 Overview Function of Components This section describes the components of the Agilent 7500 in detail and in the sequence listed below: • sample introduction • inductively coupled plasma (ICP) source • interface/vacuum • ion lenses • analyzer • detector • vacuum system • RF generator 1-12 Agilent 7500 Series ICP-MS Hardware Manual
Overview Sample Introduction Q-pole Mass Filer Sampling Cone Interface ICP Skimmer Cone Ion Lenses RF Generator 1 Analyzer EM (Electron Mutiplier) Detector Gas Controller Ar Gas Turbomolecular Pump Sample Vacuum Rotary Pump Figure 7 System Diagram (7500a) Ion Lenses Analyzer Interface Reaction Gas Q-pole Mass Filer EM (Electron Multiplier) ICP Octopole Reaction Cell Sampling Cone Skimmer Cone Figure 8 Showing differences compared to 7500a Octopole Reaction System (7500cs/cx) Agilen
1 Overview Sample Introduction The Agilent 7500 features an on- board peristaltic pump that controls the flow of sample solution into and waste (drain) out of the instrument. The peristaltic pump continuously pumps the sample solution into the sample introduction system. The solution passes into a nebulizer that disperses the sample using a stream of argon gas (Figure 9).
Overview 1 ICP Source The fine sample aerosol that exits the spray chamber passes directly into the injector tube of the horizontally mounted ICP torch. The ICP torch is comprised of three concentric quartz tubes through which streams of argon pass (Figure 10). These three gas streams are referred to as the plasma gas, auxiliary gas and nebulizer (carrier) gas.
1 Overview Interface/Vacuum System After the analyte ions are formed, they are extracted into the first vacuum stage through a hole in the front plate of the vacuum chamber referred to as the sampling cone. Ions pass through the sampling cone into the interface, which is an expansion region evacuated by a rotary pump. The ions then pass through a second orifice called the skimmer cone, which acts as a differential aperture between the interface and intermediate vacuum stage.
Overview 1 After focusing by a conventional Einzel lens, the ion beam is bent off- axis by an Omega lens, which consists of two split- ring elements that alternately repel and attract the ions. This Omega lens deflects the ion beam approximately 5 mm off- axis into the front plate of the quadrupole. Photons and neutral species are not diverted off- axis and so do not enter the quadrupole. This ensures that the system has a very low random background, resulting in excellent detection limits.
1 Overview Quadrupole The quadrupole mass analyzer consists of four long metal rods with a hyperbolic cross section which are arranged parallel to each other, and have RF and DC voltages applied to them. By varying these voltages, the rods act as a mass filter allowing only ions of a specific mass- to- charge ratio to pass through the center of the quadrupole at any given combination of applied voltages. All other masses are unstable and collide with the rods.
Overview 1 Depending on the concentration of the analytes being measured, the detector operates in one of two modes: • Pulse mode for low sample concentrations. • Analog mode for high sample concentrations. Vacuum System The sample is ionized in the plasma and the ions go through the interface, the ion lens, and the mass filter to the detector. A lower vacuum pressure in the vacuum chamber is required to transmit the ions.
1 Overview Interface Chamber The interface chamber is located between the sampling cone and the skimmer cone. A rotary pump evacuates the interface chamber. Ion Lens Chamber The ion lenses are located in the ion lens chamber. A turbomolecular pump evacuate the ion lens chamber. Analyzer Chamber The mass filter and the detector are located in the analyzer chamber. A turbomolecular pump evacuates the analyzer chamber. The rotary pump is also used for pumping the interface chamber turbomolecular pump.
Overview 1 Support Systems The Agilent 7500 requires argon, cooling water, electrical power and positive exhaust ventilation. Refer to the Agilent 7500 Series ICP- MS Site Preparation Guide for additional information. The MassHunter Workstation (or ChemStation) software controls the Agilent 7500 and interprets the resulting data. Following subsystems are water cooled.
1 Overview Peripheral Equipment The optional peripheral equipment extends the application range of the Agilent 7500. The following sections describe the available peripherals. Autosampler (I-AS) You can use the random access autosampler to analyze a sequence of samples without operator intervention. A two- channel peristaltic pump provides a flowing rinse and segmented racks allow for rack replacement during operation.
Overview 1 ISIS can be setup to perform various on- line sample introduction techniques such as: • Pre- defined application: High Sample Throughput, Auto Dilution, Discrete Sampling • Customer definable application: Hydride Generation, Matrix Elimination Laser Ablation System The Laser Ablation System provides a means of rapid, direct analysis of solid samples without dissolution and minimal sample preparation.
1 Overview Specifications The following specifications are subject to change without notice. A copy of the most recent specifications in the form of a specification sheet can be obtained from your local Agilent Technologies office. Table 2 Name Agilent 7500 Series ICP-MS (Agilent 7500) ICP Solid State System MS Frequency 27.
Agilent 7500 Series ICP-MS Hardware Manual 2 Precautions Protective Earth 2-4 Closing the Instrument Panels and Hoods 2-4 Wearing Safety Glasses 2-4 Checking the Exhaust System 2-5 Handling Solvents Correctly 2-6 Checking the Drain Vessel 2-7 Storing Argon Safely 2-8 Hydrogen (H2) Gas 2-8 Other Gas 2-10 Allowing the Hot Instrument to Cool 2-11 Torch Box Cover 2-11 Peristaltic Pump 2-11 Rotary Pump 2-11 Air Intake and Outlet 2-11 Beryllium and Beryllium Oxide 2-12 Moving the Agilent 7500 ICP-MS 2-13 Environ
2 Precautions WA R N I N G If you have a pacemaker or similar implanted device, consult your physician before using this device. This device can potentially affect pacemaker function. CAUTION The Agilent 7500 Series ICP-MS (Agilent 7500) is a very safe instrument with many built-in protective features: • A safety interlock prevents opening of the hoods during operation. • A plasma viewing window provides eye protection. • Sensors monitor the water and argon flow rate and pressure.
Precautions NOTE CAUTION 2 To shut down the instrument quickly, turn OFF the power switch located on the lower right side of the front panel. To switch the instrument to Standby mode and/or Shutdown mode without using MassHunter Workstation (or ChemStation), a “Plasma Off Switch” and “Shutdown Switch” are available on the instrument top cover. • A sensor monitors the radio frequency (RF) generator and shuts it down if it is improperly matched to the work coil.
2 Precautions Protective Earth WA R N I N G Connecting the Agilent 7500 ICP-MS to a power source that is not equipped with a protective earth contact creates a shock hazard for the operator and can damage the instrument. Likewise, interrupting the protective conductor inside or outside the Agilent 7500 ICP-MS or defeating the power cord ground creates a shock hazard for the operator and can damage the instrument.
Precautions 2 Checking the Exhaust System CAUTION Due to potential health hazards, the exhaust gases from the plasma and vacuum systems must be eliminated through the laboratory ventilation system via the instrument exhaust vent. If inadequate ventilation occurs, it will cause vaporized pump fluid, ozone, and other toxic combustion products to accumulate in the laboratory. Hydrofluoric acid (HF) fumes, if inhaled, cause extensive burning of lung tissue.
2 Precautions Handling Solvents Correctly CAUTION Organic and aqueous solvents can be hazardous if handled improperly. Always follow the precautions listed below to protect both operator and instrument: • Read the Material Safety Data Sheet (MSDS) for each solvent used. • Prepare samples and transfer acids under a fume hood with adequate extraction. • Wear gloves when handling acids or solvents. • Wear safety glasses when handling any liquids.
Precautions 2 Checking the Drain Vessel CAUTION The drain vessel contains the spray chamber effluent, which can be toxic. Improper handling of the vessel can result in a serious explosion or fire if incompatible substances are accumulated. Corrosion of the vessel and connecting tube can result in leaks that may damage the instrument or cause bodily harm.
2 Precautions Storing Argon Safely WA R N I N G Argon, which is used to create the plasma, is a dangerous gas only if it displaces the air you are breathing or is mishandled in its storage cylinder. Take the following precautions to prevent an explosion or suffocation hazard: • Secure the cylinder valve caps and move the cylinder with an approved handcart. • Label the gas cylinder clearly and store it vertically away from all ignition and heat sources.
Precautions 2 Dangers During ICP-MS Operation WA R N I N G Hydrogen presents a limitless number of dangers during ICP-MS operation. These include, but are not limited to: • Combustion from leaking hydrogen. • Combustion due to rapid expansion of hydrogen from high pressure. • Accumulation of hydrogen in the ICP-MS and subsequent combustion. Hydrogen can accumulate in the ICP-MS in a number of unstipulated or uncommon ways. All users must be aware of the mechanisms by which hydrogen can accumulate.
2 Precautions Necessary Precautions During ICP-MS Operation WA R N I N G The following are general precautions that should be taken during ICP-MS operation to prevent combustion of hydrogen gas. Other precautions may be necessary depending on the setting and configuration in which you use the system. Pay careful attention to safety management when using this system. • Make sure the hydrogen gas line is without leaks.
Precautions 2 Allowing the Hot Instrument to Cool WA R N I N G The torch and interface remain hot after the plasma is turned off. Do not touch the torch box or interface cones for 10 minutes after turning off the plasma to allow for cooling. Torch Box Cover CAUTION Attach the torch box cover after maintenance. This cover reduces the emission noise from the plasma. Peristaltic Pump CAUTION Be aware that the clamp of the peristaltic pump opens and closes.
2 Precautions Beryllium and Beryllium Oxide Product and environmental safety - toxic materials WA R N I N G There is a toxic hazard associated with parts containing beryllium. Precautions need to be observed in the handling, storage, transport and disposal of such parts. Beryllium oxide is a white powder which may be molded into shape by a sintering process to form a ceramic similar in appearance to other electrical ceramics.
Precautions 2 Moving the Agilent 7500 ICP-MS CAUTION Stated below are precautions you should observe when you want to move your Agilent 7500. • Make sure the Agilent 7500 Main Power Breaker (located on the rear side) is turned OFF before moving the Agilent 7500. • Make sure all the cables between other units are unplugged and the utility tubing are disconnected before moving equipment (small moves for adjustments etc. can be done without unplugging and disconnecting).
2 Precautions NOTE The “Installation category” implies the regulation for impulse withstand voltage. It is also called the “Over voltage category”. “II” applies to electrical equipment. “Pollution level” describes the degree to which a solid, liquid, or gas which deteriorates dielectric strength is adhering. “2” applies to a normal indoor atmosphere.
Precautions 2 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. Electrical Power (Voltage, Frequency, Amperage, Phase) 200- 240 VAC, 50/60 Hz, 30 A, single phase Argon Gas Supply Minimum Purity: Maximum Flow Rate: Supply Pressure: 99.
2 Precautions Symbols Used on the Instrument The following symbols are used on the instrument. 2-16 : To avoid personal injury, death, or damage to the instrument, the operator must refer to an explanation in the Manual. This symbol is placed on the product where it is necessary for you to refer to the manual in order to understand a hazard. : Protective grounding terminal. : Alternating current.
Precautions 2 Others Part Numbers In the Agilent 7500 Series ICP- MS Customer Maintenance Parts List, Agilent Technologies part numbers are generally listed in parentheses after the name of the part or in the tables. A few tools and supplies listed have no part number and are not available from Agilent Technologies. Most of these can be obtained from laboratory supply companies. Serial Number The Agilent 7500 ICP- MS is identified by a serial number on a label attached to the instrument.
2 2-18 Precautions Agilent 7500 Series ICP-MS Hardware Manual
Agilent 7500 Series ICP-MS Hardware Manual 3 Startup, Shutdown and Status Starting the Instrument 3-2 Shutting Down the Instrument 3-10 Checking the Instrument Status 3-13 Typical Meter Values for the Vacuum System 3-18 The Agilent 7500 Series ICP- MS is designed so that it is easy to startup and shutdown.
3 Startup, Shutdown and Status Starting the Instrument There are three states from which the Agilent 7500 can be started: • Unplugged • Shutdown mode • Standby mode This section explains how to start the instrument from all three states. Starting the Instrument from Cold Use the following procedure to startup the instrument after it has been unplugged for a move, maintenance, or a long- term shutdown. 1 Ensure that the instrument is plugged in. Plug the instrument into a NEMA L15- 30R power receptacle.
Startup, Shutdown and Status 3 Power Switches for the Rotary Pumps SERIAL A Main Power Breaker SERIAL B ETHERNET REMOTE Main Power Supply Cable Figure 14 Power Connections for the Rotary Pumps Rear View and Control Switches 5 Turn on the instrument power switch. The power switch is located on the front panel. The instrument now has power and the green light on the power switch is lit.
3 Startup, Shutdown and Status 6 Startup the printer and computer. Refer to the printer and computer user manuals for more information. 7 Start the MassHunter Workstation (or ChemStation) software.
Startup, Shutdown and Status 3 8 Select Instrument>>Instrument Control. The Instrument Control window (Figure 17) appears. The title bar shows that the instrument is in Shutdown mode. The LED located on the top right corner of the right top cover is off during Shutdown mode. Continue with “Starting from Shutdown Mode”.
3 Startup, Shutdown and Status 2 Click Yes. The instrument will turn on the rotary pump, open the backing line valve and turn on the turbo pump. The Instrument Control diagram displayed in MassHunter Workstation (or ChemStation) will indicate that the rotary pump is on. It can take from 15 minutes to 2 hours for the vacuum chamber to attain its correct pressure of 5 x 10- 4 Pa. The instrument is now in Standby mode, as displayed in the title bar.
Startup, Shutdown and Status 3 Starting from Standby Mode The following instructions assume that the instrument is in Standby mode and the analyzer vacuum chamber is evacuated to a partial or high vacuum. See “Starting from Shutdown Mode” to evacuate the vacuum chamber. The plasma is off when the Agilent 7500 is in Standby mode. At this point the Plasma can be switched on. Once the interface vacuum has reached 4.
3 Startup, Shutdown and Status CAUTION Be sure to clamp the peripump tubing from the drain in the peripump. The drainage for the spray chamber is provided by this peripump. If the spray chamber is not drained properly, it will fill with solution causing solution to flow to the torch which will cause the plasma to turn off. 8 Select Plasma>>Plasma On. A dialog box appears asking if you want to turn the plasma on. Figure 20 9 Click Yes.
Startup, Shutdown and Status Figure 21 3 Instrument Control Screen in Analysis Mode (Picture may differ depending on ICP-MS Model/Mode) WA R N I N G Flow Direction (Drain Vessel) (PeriPump) Air Waste Solution Confirm that the drain is flowing. Check that the tube from the drain peristaltic pump to the drain bottle is properly connected. You should see a regular pattern of liquid and air as shown above.
3 Startup, Shutdown and Status Shutting Down the Instrument The Agilent 7500 is in Analysis mode during tuning and sample analysis. When not being used for these procedures, the instrument remains in Standby mode. To maintain or move the instrument, it should be placed in Shutdown mode and turned off. The following sections explain how to return the Agilent 7500 to Standby mode at the end of each day and how to put the instrument in Shutdown mode when necessary.
Startup, Shutdown and Status NOTE 3 Turning off the computer and printer while the instrument is in the Standby mode will not cause any problems. Putting the Instrument in Shutdown Mode CAUTION Except in emergency situations, you should put the Agilent 7500 into the Shutdown mode before turning off the main power.
3 Startup, Shutdown and Status NOTE If argon gas is not supplied, air will be introduced into the vacuum chamber instead of argon. In this case, it may take more time to go back to Standby mode. Turning the Instrument Completely Off Turn the Agilent 7500 completely off when you want to perform maintenance on electrical components or move the instrument.
Startup, Shutdown and Status 3 Checking the Instrument Status The Agilent 7500 MassHunter Workstation (or ChemStation) software provides two methods for checking the instrument status: • Instrument Control Diagram • Meter Control Panel This section explains how to use these monitoring screens. Checking the Instrument Control Diagram The Instrument Control window is a real- time display that enables you to quickly assess the current status of the instrument.
3 Startup, Shutdown and Status The Carrier Gas Flow meter box appears. An acceptable range of values for this meter is application specific. 4 Repeat Step 3 until you have checked all 14 system components on the Instrument Control screen. Checking the Meter Control Panel MassHunter Workstation (or ChemStation) also provides a Meter Control Panel for checking the instrument’s status.
Startup, Shutdown and Status 3 2 Select Meters>>Meter Control Panel. The Meters panel appears (Figure 25). Figure 25 Meters Panel (Picture may differ depending on ICP-MS Model/Mode) 3 Select up to five components to monitor by clicking the appropriate check boxes and then clicking OK. Meter boxes for the selected components appear on the right side of the screen. Check the following table to ensure that values displayed are within acceptable limits.
3 Startup, Shutdown and Status 4 To monitor other components, deselect the current ones by clicking the appropriate boxes. Then click the boxes next to the additional components you want to monitor. Meter boxes for the newly selected components appear on the right side of the screen. 5 Repeat Step 4 until all necessary components have been checked. Table 3 Meter Control Panel Values Meter Typical Ranges Shutdown Mode Units Standby Mode Analysis Mode IF/BK Press – 0.
Startup, Shutdown and Status Table 3 Meter Control Panel Values (continued) Meter Typical Ranges Shutdown Mode Standby Mode Units Analysis Mode H2 Gas *7 0 0 3~5 mL/min *7 0 0 3~5 mL/min He Gas 3 *1 RP: Rotary Pump *2 Depending on the type and flow rate of the reaction gas used, pressure may rise out of the typical range when operating in the standard mode, He mode, or H2 mode (standard for 7500cs/ce and optional for 7500cx).
3 Startup, Shutdown and Status Typical Meter Values for the Vacuum System Refer to the following meter values when the error occurs. 1 After the vacuum is ON Table 4 Parameters Limit Conditions Backing pressure (IF/BK) > 100 Pa if BK is higher, even 60 seconds after the vacuum is ON. Backing pressure (IF/BK) > 25 Pa if BK is higher, even 70 minutes after the vacuum is ON. Analyzer pressure (AN) > 5 x 10-4 Pa if AN is higher, even 5 hours after the vacuum is ON.
Startup, Shutdown and Status 3 4 In Standby mode Table 7 Parameters Limit Conditions Analyzer pressure (AN) > 2 x 10-3 Pa Agilent 7500 goes back to Shutdown mode. Backing pressure (IF/BK) > 60 Pa Agilent 7500 goes back to Shutdown mode. 5 In Analysis mode (std) (7500cs/cx) Table 8 Parameters Limit Conditions Interface pressure (IF/BK) > 530 Pa Agilent 7500 goes back to Standby mode. Analyzer pressure (AN) > 2 x 10-3 Pa Agilent 7500 goes back to Standby mode.
3 3-20 Startup, Shutdown and Status Agilent 7500 Series ICP-MS Hardware Manual
Agilent 7500 Series ICP-MS Hardware Manual 4 Maintenance Maintenance 4-2 Scheduling Maintenance 4-3 Checking Lab Conditions 4-5 Maintenance Clocks 4-5 Maintenance Log 4-9 Fuse 4-14 Cleaning the Frame 4-14 Sample Introduction 4-14 Peristaltic Pump Tubing 4-15 Sample Line Connector Block 4-18 Internal Standard Tubing Kit 4-21 Maintaining the Nebulizer and Spray Chamber 4-25 Maintaining the Torch 4-51 Maintaining the ShieldTorch 4-59 Maintaining the Cones 4-66 Maintaining the Lenses (Agilent 7500a) 4-75 Maint
4 Maintenance Maintenance This chapter contains operator maintenance procedures for the Agilent 7500. A summary table of tasks is given, followed by the procedures by component. To repair any Agilent 7500 component not listed, call your Agilent Technologies service representative. For maintenance of the computer workstation or a peripheral, refer to the hardware manuals for that equipment. Each maintenance procedure is prefaced by a list of necessary tools and supplies.
Maintenance 4 Scheduling Maintenance Table 9 Maintenance Schedule Frequency Component Daily Argon gas (As a matter of routine, check daily before starting work and Drain vessel over the course of daily analysis) Task/Action Check argon gas pressure and volume Check, empty if required Peristaltic pump tubing Check for damage/deterioration Weekly Sampling cone, Skimmer cone Check orifice for foreign matter, deformation and enlargement Monthly Rotary pump Check oil level and color.
4 Maintenance Table 9 Maintenance Schedule (continued) Frequency Component Task/Action Periodically (Maintenance frequency of these components is highly dependent on lab conditions and sample throughput.
Maintenance 4 Checking Lab Conditions You must maintain the environmental conditions required by the Agilent 7500 which were established during installation, because they can affect both safety and instrument performance. For additional information, refer to the Chapter 2 and the Agilent 7500 Series ICP- MS Site Preparation Guide. Maintenance Clocks Use the MassHunter Workstation (or ChemStation) software to help determine your maintenance schedule.
4 Maintenance Viewing the Maintenance Clocks To check the maintenance counter and clocks, complete the following steps: 1 Select Instrument>>Instrument Control from the ICP- MS Top window. The Instrument Control window appears. 2 Select Diagnostics>>Running Time. The Running Time dialog box appears. See on- line help for additional information on each value displayed.
Maintenance 4 3 Check the Current Time (or EM Total Current). The lapse of time displayed in the Vacuum Running Time area means the cumulative time of vacuum operation (Standby mode and Analysis mode). The lapse of time in the Plasma Running Time area means the cumulative time of plasma ignition (Analysis mode). Both areas show the lapse time from the last click of the Reset button until the present time.
4 Maintenance Setting the Maintenance Period If the maintenance items and maintenance periods are set beforehand, it is possible to display the message telling the maintenance time based on the total time of igniting the plasma, operating the vacuum, and the lapse of time. To set the maintenance period, complete the following steps: 1 Input the period of time in the Maintenance Period textbox. 2 Click the checkbox to the left to display a check in it.
Maintenance 4 Maintenance Log It is possible to record the tuning parameters, the tuning report, and all the parameters regarding the instrument condition in the maintenance logbook. You can also add maintenance records and comments in the logbook. The logbook is saved in the below directory.
4 Maintenance To change the displayed items, complete the following steps: 1 Click the item area above the Maintenance LogBook window. The Change List Item dialog box appears. Click here Figure 29 The displayed item area of the Maintenance LogBook window Figure 30 Change List Item Dialog Box. 2 Select the Tune report or Meter Value in the Category area and choose the item in the column below. Click OK, then the selected item appears in the Maintenance LogBook window.
Maintenance 4 Recording the Maintenance Log When the maintenance logs are recorded, current meter values and the last tuning report are recorded. To record the maintenance logs, complete the following steps: 1 Click Record Log in the Maintenance LogBook window. The Logbook Editor dialog box appears. Figure 31 Logbook Editor dialog box 2 In the Logbook Editor, if there are maintenance items to be done at this time, click the check boxes. You can also type comments to record in the logbook.
4 Maintenance The Maintenance Log Display Use the Logbook Viewer dialog box to examine each recorded maintenance log. To display the maintenance logs, complete the following steps: 1 Choose and click the log item to be displayed in the Date Logged of the Maintenance LogBook window, and click View Log (Figure 28). The Logbook Viewer dialog box appears. Figure 32 NOTE 4-12 Logbook Viewer Dialog Box You can also display the Logbook Viewer by double clicking the date.
Maintenance 4 2 Check the contents of the logbook. The following content appears when selecting each menu. • Tune Tuning parameters and tuning results are displayed. • Logs>>View ACQ Log Data acquisition log is displayed. • Logs>>View Sequence Log Sequence log is displayed. • Logs>>View Chained Seq Log Chained sequence log is displayed. • Logs>>View Error Log Error log is displayed. • View Maintenance Records Maintenance items selected in the check box of Logbook Editor dialogue box appears.
4 Maintenance Fuse The fuse is not replaceable by the user because it is inside of the enclosure. If you believe the fuse is blown, please contact your local Agilent Technologies office. Cleaning the Frame When the surface of the Agilent 7500 Mainframe becomes dirty, wipe it with a dry cloth. Sample Introduction • Replacing the peristaltic pump tubing. • Cleaning and exchanging of the nebulizer, spray chamber, and end cap. It is important to always keep the sample introduction parts clean.
Maintenance 4 Peristaltic Pump Tubing When the peristaltic pump (peripump) no longer pumps the sample with an even flow, wash or replace the pump tubing or readjust the pump clamps. Change the peristaltic pump tubing in the following cases. • When the tubing becomes too loose to uptake a solution. • When the inside of the tubing is damaged and dregs are released. • When it is impossible to remove sample memory. This is especially important if you keep using old tubing.
4 Maintenance Replacing the Peristaltic Pump Tubing To replace the peristaltic pump tubing, complete the following steps: WA R N I N G When replacing the peristaltic pump tubing, stop the pump rotation before disassembling. Before changing the peristaltic pump tubing, replace the solution in the tubing to water. 1 Place the instrument in Standby mode. See Chapter 3, “Startup, Shutdown and Status” to turn off the plasma, which puts the instrument in Standby mode.
Maintenance 4 3 Installing tubes on the peristaltic pump. 1 Connect a sample tube from both ends of the pump tube. 2 Referring to Figure 34, install the combined tube in the peristaltic pump. Based on the direction of the peristaltic pump rotation, hang one stopper on the pump. Stretch the tube to bring it into close contact with the roller and hang the other stopper on the pump. 3 Clamp the tubes in place.
4 Maintenance WA R N I N G Flow Direction (Drain Vessel) (PeriPump) Air Waste Solution Confirm that the drain is flowing. Check that the tube from the drain peristaltic pump to the drain bottle is properly connected. You should see a regular pattern of liquid and air as shown above. Sample Line Connector Block The action of the peristaltic pump rollers on the pump tubing can generate static electricity in dry atmospheric conditions.
Maintenance 4 To attach this connector, complete the following steps: 1 The connector block is shown in the following figure. The connector block (black) is made of an electrically conductive polymer, which grounds the sample solution to the chassis via a fine Pt wire. The Pt wire just protrudes through the end of the connector, making contact with the sample. Teflon Tubing Teflon Tubing from Nebulizer 0.5-1.
4 Maintenance 5 Complete steps 2- 4 for both the tube from the nebulizer and the supplied sample tube. NOTE Connect the peristaltic pump tube to the opposite end of the supplied sample tube. 6 Clip the block into the ground clamp. The conducive connector fits in the ground clamp, making an electrical contact between the sample and the chassis. Check for leaks.
Maintenance 4 Internal Standard Tubing Kit This kit is for on- line addition of internal standard solution. Please refer to the following description for this kit prior to use. The connector block is made from high- purity materials, which have been thoroughly tested by Agilent, and no sample contamination has been observed. The block has a very small dead volume (1 micro liter), minimizing sample washout time. This kit also serves as the “sample line connector block” at the same time.
4 Maintenance To attach this kit, complete the following steps: 1 Perform the following procedure to connect the tube adapter and pump tube. 1 Cut the pump tube diagonally and moisten with pure water. 2 Insert the moistened pump tubing into the Teflon tubing until it is fed completely through. 3 Cut the pump tubing together with the Teflon tubing. If the tubes are not cut at a 90- degree angle, a leakage or blockage may occur in the connector.
Maintenance 4 2 Perform the following procedure for non- pump tube connections. 1 Cut the ends of the tubing at a 90- degree angle to prevent leakage or blockage. 2 Slide a Teflon nut, back ferrule and front ferrule on to the tubing. The tubing should protrude between 0.5 and 1.0 mm beyond the front ferrule. F ront & Back Ferrule Teflon tubing Teflon Nut 0.5-1.0 mm Figure 41 Teflon Nut, Front and Back Ferrule 3 Insert the end of the Teflon tubing into the connector block as far as possible.
4 Maintenance NOTE Excessive tightening will cause leakage and clogging in the connector. 3 Connect 3- way Connector Block, Peristaltic Pump Tubing, Internal Standard Tubing Kit, etc.
Maintenance 4 Maintaining the Nebulizer and Spray Chamber The nebulizer and spray chamber need to be cleaned if memory effects are observed after running high matrix samples, or when ultimate detection limits (ppt) are necessary. The nebulizer and spray chamber are located in the open area of the sample introduction part on the left of the instrument. The spray chamber is tilted to facilitate drainage.
4 Maintenance WA R N I N G NOTE • Use organic solvent such as acetone and methanol in a well-ventilated place like the draft. • Handle acid carefully. Pure water used for cleaning is indicated as water that has been generated using the ion-exchange method and a membrane filter, and has an electrical resistance of at least 18 MΩ.
Maintenance 4 Top Cover Connector Tube Ball Joint Clamp Spray Chamber Nebulizer and End Cap Spray Chamber Chiller Figure 44 Nebulizer, Spray Chamber and Spray Chamber Chiller To remove and check the nebulizer and spray chamber, complete the following steps: 1 Put the instrument in Standby mode. See Chapter 3, “Startup, Shutdown and Status”. 2 Remove the sample transfer line. Remove the ball joint clamp and disconnect the connector tube (Figure 44).
4 Maintenance 3 Disconnect and check the gas hoses and sample tube. Remove the quick- connect fittings. Carefully twist the hoses off the end cap and nebulizer (Figure 44). If makeup gas is being used, remove that clamp and hose. Otherwise, unscrew the gas plug and disconnect the sample tube. As you remove the gas hoses and the sample tube, check them for damage such as splitting, pinches or deterioration. Replace if needed. 4 Remove the spray chamber retaining bracket.
Maintenance 4 Cleaning the Babington Nebulizer and the End Cap The carrier gas pressure is generally 500 to 600 kPa at a 1.2 L/min carrier gas flow rate.The argon gas supply pressure has to be set to 700 kPa. If carrier gas pressure rises to more than 600 kPa, the nebulizer may become clogged.
4 Maintenance To clean a clogged nebulizer, complete the following steps: 1 Pump 5% Nitric Acid through the nebulizer for 10 minutes while it is still attached to the spray chamber. Wear safety glasses and gloves when working with acid. 2 If this does not remove the material clogging the nebulizer, remove the nebulizer from the end cap. The sample uptake tube can remain on the nebulizer.
Maintenance 4 To resolve signal instability, complete the following steps: 1 Remove the nebulizer and end cap. The sample uptake tube can remain on the nebulizer. Refer to the “Disconnecting the Babington Nebulizer from the End Cap” Remove the O- ring before soaking the nebulizer in acetone. Once the O- ring is soaked in acetone, it will swell and installation will be difficult. 2 Soak the nebulizer for 10 minutes in acetone. 3 Soak the nebulizer for 10 minutes in methanol.
4 Maintenance To solve memory problems, complete the following steps: 1 Disconnect the nebulizer and the end cap. The sample uptake tube can remain on the nebulizer. Refer to the “Disconnecting the Babington Nebulizer from the End Cap” 2 Ultrasonic the nebulizer in 5% Nitric Acid. Wear safety glasses and gloves when working with acid.
Maintenance 4 Disconnecting the Babington Nebulizer from the End Cap NOTE Wear gloves when handling the Babington nebulizer to avoid getting oils from your hands on the surface of nebulizer. If contaminated with oil, wetability of the surface of the nebulizer is compromised and the signal becomes unstable. The wetability of spray surface of the Babington nebulizer is significant for the signal stability.
4 Maintenance Thumb Screws Removal Tool Sample Tubing Plate Babington Nebulizer End Cap Connection Port for Make-up Gas Figure 46 3 Remove the two O- rings. 4 Complete following steps to disconnect the sample uptake tube with the tube adapter if there is a memory problem: a Insert the groove of the attachment tool between the tube connector and the nebulizer body. Refer the following figure.
Maintenance 4 Teflon Tubing Tube Connector Attachment Tool Babinton Nebulizer Figure 48 NOTE Disconnecting the Tube Connector Do not disconnect the Teflon tubing from the tube connector unless there is a heavy memory problem or the tip is broken. 5 Check the O- ring in the end cap.
4 Maintenance Reattaching the Babington Nebulizer and the End Cap CAUTION Wear gloves when handling the Babington nebulizer or the sample tube to avoid getting oils from your hands on the surface of nebulizer. If contaminated with oil, the wetability of the surface of the nebulizer is compromised and the signal becomes unstable. Also, the spray part of the nebulizer is delicate. Do not touch. 1 Reconnect the sample uptake tube if it has been removed.
Maintenance 4 3 Place the sample uptake tube end on a clean plane vertically as shown the following figure. 4 Slide the tube connector toward the clean plane gently so that the edges of the sample uptake tube and the tube connector are flush with each other. Refer to the following figure. Be careful not to handle the tip with force, or it may become disfigured. Place the tube end on the clean plane vertically. Tube Connector Clean Plane Slide the connector.
4 Maintenance Gently push the nebulizer into the end cap making sure that the alignment pin fits into the slot on the back of the end cap. The tip of the nebulizer protrudes through the front of the end cap. Adding a few drops of pure water will ease insertion. NOTE There is a dedicated end cap for the Babington Nebulizer. The Babington Nebulizer has an alignment pin and the end cap has a slot into which the alignment pin fits.
Maintenance 4 Cleaning the Concentric Nebulizer, MicroMist Nebulizer and the End Cap NOTE Maintenance for the MicroMist Nebulizer is same as the Concentric Nebulizer. The carrier gas pressure is generally 200 to 300 kPa at a 1.0 L/min carrier gas flow rate. The argon gas supply pressure has to be set to 700 kPa. If the carrier gas pressure rises to more than 300 kPa, the nebulizer may become clogged.
4 Maintenance Tubing for Make-up Gas End Cap O-ring Tubing for Carrier Gas Nebulizer Teflon Tubing for Sample Figure 53 MicroMist Nebulizer and End Cap To clean a clogged nebulizer, complete the following steps: 1 Disconnect the nebulizer from the end cap. Refer to “Disconnecting the Concentric Nebulizer and the End Cap”. 2 Wash the nebulizer by pumping pure water through the nebulizer in the opposite direction. Reverse the sample tubing on the peripump and place the nebulizer tip in pure water.
Maintenance 4 If the signal is unstable, clean the nebulizer in the following way: 1 Disconnect the nebulizer from the end cap. Remove the O- rings. Refer to the “Disconnecting the Concentric Nebulizer and the End Cap” Remove both the sample tube and the connector as well. 2 Soak the nebulizer in 5% Nitric Acid both overnight. Wear safety glasses and gloves when working with acid. 3 Check the O- rings.
4 Maintenance If there is a memory, clear it by completing the following steps: 1 Disconnect the nebulizer from the end cap. Remove the O- rings. Refer to “Disconnecting the Concentric Nebulizer and the End Cap”. Disconnect the sample tube and the connector as well. 2 Soak the nebulizer in 5% Nitric Acid both overnight. Wear safety glasses and gloves when working with acid. 3 Check the O- ring. Check the O- ring used as the connector between the sample line and the carrier gas.
Maintenance 4 Replacing or Refitting the Concentric Nebulizer and the End Cap 1 Reinsert the nebulizer into the end cap. Replace the two O- rings in the hole in the center of the end cap. Install the nebulizer holder nut on to the end cap first. At this time, do not tighten it. Insert the nebulizer through the nebulizer holder nut and then insert the nebulizer into the O- rings by gently applying pressure and twisting the nebulizer.
4 Maintenance Cleaning the PFA Concentric Nebulizer The carrier gas pressure is generally 200 to 300 kPa at a 1.0 L/min carrier gas flow rate. The argon gas supply pressure has to be set to 700 kPa. If the carrier gas pressure rises to more than 300 kPa, the nebulizer may become clogged. CAUTION A wire or similar material must not be used to clear a clogged concentric nebulizer or the nebulizer will be damaged and may be rendered unusable.
Maintenance 4 When Blockage Occurs When blockage is evident please clean following the method below. If washing with the below method does not clear the blockage, please replace the PFA concentric nebulizer. When removing the nebulizer from the end cap, please also inspect the O- ring. If there is any deterioration please replace the O- ring. 1 Disconnect the nebulizer from the end cap.
4 Maintenance Removing the PFA Concentric Nebulizer 1 Loosen the union connector which connects the carrier gas tube and remove the tube. 2 Remove the nebulizer. Loosen the nebulizer holder nut and gently pull the nebulizer out of the end cap while gently twisting it. Take care not to touch the nebulizer tip against the inside wall of the end cap. 3 When removing the nebulizer, also remove the end cap and inspect the O- rings between the end cap and spray chamber for deterioration or damage.
Maintenance 4 Makeup Gas Connecter End Cap Nebulizer Holder Nut PFA Concentric Nebulizer Carrier Gas Connecter Figure 56 Nebulizer Orientation Cleaning the Spray Chamber and the Transfer Line To clean the spray chamber and the transfer line, complete the following steps: CAUTION • Do not use chemicals such as Hydrofluoric Acid (HF), which erodes quartz, to clean the spray chamber. • An ultrasonic wash must not be used to clean spray chambers that are made of quartz.
4 Maintenance CAUTION TMAH and ammonia water are basic reagents. Be sure to wear gloves when handling them. Do not mix basic reagents such as TMAH and ammonia water with acidic reagents such as nitric acid and hydrofluoric acid. Be sure to fully rinse parts soaked in basic reagents with pure water before use. 1 Remove the transfer line and the spray chamber from the end cap. Refer to the “Removing and Checking the Nebulizer and Spray Chamber”. 2 Thoroughly wash with pure water. 3 Soak in 5% Nitric Acid.
Maintenance 4 Replacing or Refitting the Nebulizer and Spray Chamber Before reconnecting the gas hoses, reattach the nebulizer and spray chamber. Replace these components if they are cracked or broken. To refit the nebulizer and spray chamber, complete the following steps: 1 Fit the end cap onto the spray chamber. See Figure 44. Push the end cap onto the spray chamber until there is a snug fit and the makeup gas fitting is perpendicular to the ball joint fitting.
4 Maintenance 3 Reconnect the sample and gas tubing. Use the figures of each nebulizer to identify the sample introduction hose and gas hoses. Connect and fasten each hose onto its fitting. CAUTION Do not over-tighten the nuts or the quick-connect clamps. The glass will break if too much pressure is applied. a Connect the sample uptake tube. Attach the sample tube from the uptake channel of the peristaltic pump to the end of the nebulizer. b Connect the carrier gas hose.
Maintenance 4 Maintaining the Torch Replace the torch whenever you notice that it is chipped, cracked, or distorted from overheating. Replacement is also necessary when the central tube of torch is deformed or clogged. Clean the torch when ultra low levels (ppt) need to be analyzed. Any white deposit in the inner tube also indicates a need for maintenance. CAUTION Slight deformation of the torch may not cause any problems.
4 Maintenance Removing and Checking the Torch To remove the ICP torch, complete the following steps: 1 Put the instrument in Standby mode. See Chapter 3, “Startup, Shutdown and Status”. WA R N I N G To avoid burns, wait 10 minutes after switching off the plasma before opening the instrument. The plasma reaches temperatures as high as 8000 K. 2 Open the torch box. Open the cover, loosen the torch box screws and remove the torch box. Remove the connection tube.
Maintenance 4 Torch Stand Hole Torch Projection (for Torch Stand) Torch Stand Torch Long base leg Figure 58 ICP Torch Agilent 7500 Series ICP-MS Hardware Manual 4-53
4 Maintenance 6 Examine the torch. Examine the torch for wear and contamination. Replace it if you find cracks, chips, or evidence of distortion due to overheating. Install the joint connecting tube between the spray chamber and the torch. Tighten the spray chamber hold down screw and replace the two ball joint clamps. Close the torch box cover and tighten the thumb nut to secure the cover.
Maintenance 4 Cleaning the Torch To clean the torch, complete the following steps: 1 Soak the torch in a 5% Nitric Acid bath overnight. Remove air bubbles trapped under the torch by slightly tipping the torch from side to side. Protective gloves and safety precautions should be observed at all time when working with Nitric acid. NOTE • Do not use HF to clean the torch as it will damage the torch. • Do not place the torch in an ultrasonic bath. 2 Rinse the torch with pure water.
4 Maintenance Refitting the Torch To place the torch back in the instrument, complete the following steps: 1 Place the torch in its holder. With the auxiliary gas fitting on top of the torch, carefully slide its open end inside the work coil and at the same time align the projection for the torch stand into the torch stand hole. Refer to Figure 58 showing how the projection for torch stand aligns with the torch stand hole.
Maintenance 4 2 Attach the hoses. After connecting the gas hoses, tighten the nuts on the fittings. See Figure 59 to correctly identify the gas hoses. To connect the gas hoses to the torch, complete the following steps: CAUTION Do not over-tighten the nuts on the quick-connect clamps. If you apply too much pressure, the torch will break. a Attach the sample transfer tube (connector tube). Connect the sample transfer tube from the spray chamber to the fitting on the end of the torch.
4 Maintenance Testing the Torch Perform the basic test after maintenance. See “Testing After Maintenance” at the end of this chapter. When the plasma is ignited, observe it through the tinted (UV protection) window to check the shape of the flame. If the gas pressures are too low, put the instrument in standby move and wait 10 minutes before checking the connections for leaks.
Maintenance 4 Maintaining the ShieldTorch Check the torch, shield plate, and bonnet according to the following criteria and perform maintenance as necessary.
4 Maintenance Removing the ShieldTorch To remove the shield torch, complete the following procedure: 1 Put the Agilent 7500 into Standby (or Shutdown) mode. WA R N I N G To avoid burns, wait 10 minutes after switching off the plasma before opening the instrument. The plasma reaches temperatures as high as 8000 K. 2 Open the torch box. Open the cover, loosen the torch box screws and remove the torch box. Remove the connection tube.
Maintenance 4 6 Disassemble the torch, shield plate, and bonnet.
4 Maintenance Cleaning the Torch To clean the torch, complete the following steps: 1 Soak the torch overnight in 5% nitric acid. When soaking the torch in nitric acid, gently rock the torch from side to side to remove air bubbles trapped inside. Wear gloves when handling nitric acid. CAUTION Do not apply chemicals such as HF to the glass. Do not use an ultrasonic bath. 2 Rinse the torch with pure water. Rinse the torch at least 3 times with pure water. Place on a clean surface to dry. 3 Dry the torch.
Maintenance 4 Assembling the Torch, Shield Plate, and Bonnet To assemble the torch, the shield plate, and the bonnet, complete the following steps: 1 Insert the torch into the shield plate. Insert the torch into the shield plate. Adjust the projection of the torch into the hole of the shield plate. Shield Plate Bonnet Projection for Torch Stand Hole Projection for Shield Plate Torch Figure 63 Torch, Shield Plate and Bonnet 2 Insert the torch and the shield plate into the bonnet.
4 Maintenance Clean the Ignition Terminal and Shield Contact Area Before installing the shield torch, clean the metallic surface that contacts the torch mounting assembly ignition terminal and shield plate as necessary. 1 Moisten a cotton swab with methanol (HPLC grade). 2 Wipe the metallic surface that contacts the ignition terminal and shield contact plate. Installing the ShieldTorch System To install the ShieldTorch, complete the following steps: 1 Place the torch in its holder.
Maintenance 4 2 Attach the hoses. After connecting the gas hoses, tighten the nuts on the fittings. See Figure 59 to correctly identify the gas hoses. To connect the gas hoses to the torch, complete the following steps: CAUTION Do not over-tighten the nuts on the quick-connect clamps. If you apply too much pressure, the torch will break. a Attach the sample transfer tube (connector tube). Connect the sample transfer tube from the spray chamber to the fitting on the end of the torch.
4 Maintenance CAUTION The torch cover must be on while using the torch. This cover reduces the emission of noise from the plasma. Maintaining the Cones Clean the cones when there are deposits on the orifice or the orifice is discolored. Because of its proximity to the torch, the sampling cone needs cleaning more frequently than the skimmer cone.
Maintenance NOTE 4 Pure water used for cleaning is indicated as water that has been generated using the ion-exchange method and a membrane filter, and has an electrical resistance of at least 18 MΩ. Removing the Cones CAUTION The platinum skimmer cone should only be used with the brass skimmer base. This allows the cone to operate at a lower temperature than with the standard stainless steel skimmer base, extending the life of the cone.
4 Maintenance 4 Move the torch box assembly to its maintenance position using the MassHunter Workstation (or ChemStation) software. To move the torch box assembly to its maintenance position, complete the following steps: a Select Instrument>>Instrument Control from the ICP- MS Top window. The Instrument Control window appears. b Select Maintenance>>Sample Introduction. The Sample Introduction Maintenance dialog box appears (Figure 66).
Maintenance 4 5 Remove the sampling cone. Insert the sampling cone wrench into the sampling cone’s exterior holes (Figure 67). Rotate the wrench counterclockwise to loosen the cone. Unscrew the cone by hand and remove it, holding it by its perimeter. CAUTION Do not touch the sampling cone orifice. Even slight pressure can damage the orifice. Loosen the sampling cone by holding it firmly. Figure 67 Removing the Sampling Cone 6 Pull and remove the sampling cone slowly to the axis.
4 Maintenance Figure 68 Removing the Skimmer Cone Cleaning the Cones Each cone must retain the shape of its orifice to be effective during analysis. Hold each cone by its perimeter and use only light pressure with your hand as you clean the orifice. There are 4 cleaning steps, the first two of which should remove normal contamination. Perform the cleaning step that is appropriate for the level of contamination.
Maintenance 4 To clean the cones, complete the following steps: 1 Check and clean the O- ring. Remove the sampling cone O- ring, which is in the interface opening. If the O- ring is cracked, replace it. If it is dirty or very dry, then wipe it with pure water. CAUTION Do not put grease on the O-ring of the sampling cone. 2 Clean with pure water (Step 1) 1 Dip a cotton swab in pure water and clean both sides of the cone. Hold the cone by its outer perimeter.
4 Maintenance Check the Orifice Retaining the correct shape and size of each orifice is critical for accurate analysis results. Ensure that the orifice diameter and the orifice shape of both the sampling cone and the skimmer cone have not changed. Use a 10x- magnifying lens to check the cone orifice. If the sampling cone's orifice is larger than 1.0 millimeters, replace the cone. If the skimmer orifice is larger than 0.4 millimeters, replace the cone.
Maintenance 4 To reattach the skimmer cone and sampling cone, complete the following steps: 1 Reattach the skimmer cone. Using the skimmer wrench, screw the skimmer cone into the interface opening. Tighten the cone with the skimmer wrench (Figure 68). CAUTION If the sampling cone and the skimmer cone are not tightly installed in the base, the skimmer cone is not cooled, the tip melts, or the vacuum does not reach the standard value and it cannot change to Standby mode.
4 Maintenance 5 Place the O- ring in the gap on the interface. 6 Replace the sampling cone on the interface. Turn by hand until tight. Be careful not to allow the cone to drop. Use your other hand to support the cone. 7 Using the supplied sampling cone removal tool, tighten to the position indicated by the mark (Figure 69). 3 Move the torch box back to the original position, install the torch box cover, and close the cover. CAUTION Attach the torch box cover after maintenance.
Maintenance 4 Maintaining the Lenses (Agilent 7500a) There are two sets of lenses in the Agilent 7500a. These are the extraction lenses and the main lens assembly, which is comprised of the Einzel lens and the Omega lens. In this procedure both sets of lenses are removed and dismantled before cleaning each lens element individually. However, each lens assembly can be cleaned separately. It is critical to reassemble the ion lenses in exactly the same order as before dismantling.
4 Maintenance To minimize maintenance time, clean the Einzel lens and Omega lens first. After cleaning the lenses and while pumping down, clean the extraction lens. While cleaning the Einzel and Omega lens, replace the vacuum cover and allow the instrument to pump down. CAUTION Switch off the Agilent 7500 power when opening the ion lens chamber and analyzer chamber for cleaning ion lenses and performing maintenance. Maintenance is performed on the following ion lenses.
Maintenance 4 * Use clean and degreased tools. * Use gloves that are powder- free and tolerant to acetone. NOTE CAUTION Pure water used for cleaning is indicated as water that has been generated using the ion-exchange method and a membrane filter, and has an electrical resistance of at least 18 MΩ. • The parts in the vacuum chamber don't like stains. Be sure to wear clean gloves and handle them in a dust-free place. • Work in a well-ventilated place due to the use of organic solvents.
4 Maintenance Vent Valve Figure 70 Vent Valve 3 Unscrew the vacuum cover. Using an Allen wrench, unscrew the cover while waiting for the pressure to equalize (this may take up to 5 minutes). 4 When the pressure is equalized, open the cover. After the hissing sound is finished, open the cover of the vacuum chamber. 5 Refit the vacuum vent valve. Screw the vent valve back into the side of the vacuum chamber. 6 Place the cover on the vacuum chamber unless working inside it.
Maintenance 4 Sealing the Vacuum Chamber and Pumping Down the System Always wear gloves when working with an open vacuum chamber. To correctly seal the vacuum chamber, complete the following steps: 1 Check and clean the O- ring. Replace the O- ring if it is cracked or compressed. Otherwise, wipe it with pure water. 2 Place the O- ring on the vacuum chamber. Fit it snugly into the groove on the top of the chamber. 3 Check and clean vacuum chamber.
4 Maintenance Removing the Extraction Lenses The two extraction lenses are located through the interface behind the skimmer cone. The sampling and skimmer cones must be removed before removing the extraction lens assembly. NOTE CAUTION This procedure assumes the instrument is in Standby mode and that the cones have been removed. To remove the cones, see “Maintaining the Cones” earlier in this chapter. Disassemble in a dust-free place.
Maintenance 4 2 Remove the extraction lens assembly. Using an Allen wrench, loosen the three screws from the skimmer base. Wearing gloves, pull the lens assembly, including the base, out of the instrument and set it down on a clean surface. 3 Disassemble the extraction lens assembly. Disassemble the lens assembly so the orientation matches the following diagram.
4 Maintenance Removing the Einzel Lens - Omega Lens Assembly The Einzel lens - Omega lens assembly is positioned inside the intermediate section of the vacuum chamber behind the extraction lenses (Figure 73). The slide valve moves between these two sets of lenses to seal the vacuum chamber. Screw 1 Screw 2 Einzel Lenses - Omega Lenses Assembly Figure 73 CAUTION 4-82 Einzel Lens - Omega Lens Assembly Disassemble in a dust-free place.
Maintenance 4 To remove the Einzel lens - Omega lens assembly, complete the following steps: 1 Shut down the Agilent 7500. See Chapter 3, “Startup, Shutdown and Status” in this manual. WA R N I N G This procedure exposes you to the high voltages of the Agilent 7500, which can be lethal. Shut the instrument down completely before proceeding. 2 Vent the analyzer vacuum and remove the vacuum cover. See “Working Inside the Vacuum Chamber” earlier in this chapter.
4 Maintenance 4 Disassemble the Einzel lens - Omega lens assembly. Disassemble the lens assembly so the orientation matches the following diagram.
Maintenance 4 Removing Plate Bias Lens The plate bias lens is located between the Einzel lens- Omega lens assembly and the quadrupole mass filter. (Figure 75) Plate Bias Lens QP Focus Guide Screw 1 Figure 75 CAUTION Position of Plate Bias (after removing Einzel lens-Omega lens assembly) Disassemble in a dust-free place. It is necessary to remove the Einzel lens- Omega lens assembly before removing the plate bias lens.
4 Maintenance 2 Remove the plate bias lens. Remove the screw fixing the plate bias lens and the QP focus guide (Screw 1), and remove the QP focus guide and the plate bias (Figure 76). Put the plate bias lens on a clean surface. Put the cover on the vacuum chamber after removing the lens. Plate Bias Lens QP Focus Guide Screw 1 Figure 76 Plate Bias Lens Cleaning the Lenses The extraction, Einzel, Omega, and plate bias lenses can be cleaned separately or together.
Maintenance CAUTION 4 When cleaning a lens it is especially important to thoroughly polish the holes where the ions will pass through. Do not polish the flange surface of the skimmer base. 2 Polish each lens orifice. Polish the orifice of each lens with alumina abrasive powder. 3 Wash and rinse each lens. First, wash the polished lenses with plenty of pure water. Ultrasonic the lenses in a 2% detergent solution for 5 minutes.
4 Maintenance Refitting the Plate Bias Lens To install the Plate Bias Lens in the vacuum chamber, start with the plate bias lens. This must be installed before installing the Einzel lens- Omega lens assembly. Otherwise, it will be impossible to install the plate bias lens. To install the plate bias lens, wear gloves and complete the following steps: 1 Install the plate bias lens and the QP focus guide to the vacuum chamber. Install the plate bias lens in the orientation as shown in Figure 76.
Maintenance 4 • QP focus (back) • QP focus (front) • Spacer 1 • Omega bias (back) • Spacer 1 • Omega(+), Omega(- ) • Spacer 1 • Omega bias (front) • Spacer 1 • base plate • Spacer 3 • Spacer 1 • Einzel Lens 3 • Spacer 1 • Einzel Lens 2 • Spacer 1 • Einzel Lens 1 NOTE The Einzel Lens 2 and the Einzel Lens 3 are the same part. 3 Tighten Screw 1 slowly. Tighten Screw 1, then unscrew about 1 turn. Be careful not to tighten too firmly, as it may become impossible to install other parts after this.
4 Maintenance 7 Test the electrical resistance of this compound lens with an Ohm meter before continuing. Ensure continuity between the Omega bias (front) and Omega bias (back), QP focus (front) and QP focus (back), and the base plate and spacer 3. Also ensure that there is no continuity between the base plate (ground) and each electrode. 2 Attach the Einzel Lens - Omega lens assembly into the instrument. Remove the vacuum chamber cover.
Maintenance 4 Testing the Lenses Perform the basic test after maintenance. See “Testing After Maintenance” at the end of this chapter. If the analyzer vacuum does not achieve its correct level (< 6 x 10- 4 Pa), check that the lenses are attached tightly enough to seal with the vacuum chamber. Maintaining the Lenses (Agilent 7500cs or 7500cx) The Agilent 7500 models are categorized in the following table based on the configuration of the ion lenses used.
4 Maintenance The Agilent 7500cs or 7500cx Main Lens assembly consists of 2 ion lens assemblies: the Extraction Lens- Omega Lens assembly and the Reaction Cell assembly. The Extraction Lens- Omega Lens assembly consists of the Extraction Lens and the Omega Lens. The Extraction Lens- Omega Lens and Reaction Cell assemblies can be cleaned separately. The ion lenses must be reassembled in their original configuration after cleaning.
Maintenance 4 Perform maintenance on the following ion lens: • Extraction Lens- Omega Lens assembly • Reaction cell assembly Locating Tools and Supplies You will need the following equipment when maintaining the ion lenses: • Safety glasses • Pure water • 2% detergent solution • Methanol (HPLC grade) or acetone (EL grade) for cleaning the tools • Polishing paper (#400, #1200 grit P/N: G1833- 65404) • Laboratory gloves • Allen wrench (included in the tool kit) • Jewel driver (Phillips) • Ultrasonic bath •
4 Maintenance Working Inside the Vacuum Chamber The vacuum chamber must be completely sealed to achieve high vacuum required by the Q- pole. Poor vacuum will affect its performance. This procedure explains how to break vacuum and how to achieve a good vacuum after the chamber has been opened. The vacuum chamber must be kept clean by wearing laboratory gloves while performing maintenance. When you are not working directly inside the vacuum chamber, keep the cover on.
Maintenance 4 3 Remove the screws that secure the upper cover of the vacuum chamber. While waiting for the vacuum chamber pressure to equalize, use an Allen wrench to remove the screws on the upper cover. It will take approximately 1 minute for the chamber pressure to equalize. 4 Once the vacuum chamber has equalized, remove the cover. When the vacuum chamber pressure has equalized, the soft hissing noise of air flowing into the chamber will stop. 5 Refit the vent valve.
4 Maintenance 4 Close the cover on the vacuum chamber. Place the cover on the vacuum chamber and secure the screws in sequence, working from one side to the other with the Allen wrench. 5 Make sure the vacuum vent valve is closed. Re- check the vent valve to make sure it is securely tightened. 6 Close the hoods. 7 Pump down the system. • Turn on the power. • Re- start the ICP- MS Top window from MassHunter Workstation (or ChemStation).
Maintenance 4 Removing the Extraction Lens-Omega Lens Assembly The Extraction Lens- Omega Lens assembly is located through the interface behind the Skimmer Cone. The Sampling and Skimmer Cones must be removed before removing the Extraction Lens- Omega Lens assembly. NOTE This procedure assumes that the Agilent 7500 is in Standby mode and the Sampling and Skimmer Cones have been removed. For information on removing the Sampling and Skimmer Cones, refer to “Maintaining the Cones” in the previous section.
4 Maintenance The following procedure describes how to remove the Extraction Lens- Omega Lens assembly: 1 Locate the Extraction Lens- Omega Lens assembly. The Extraction Lens- Omega Lens assembly is located behind the skimmer cone (refer to Figure 78 for the 7500cx and Figure 79 for the 7500cs).
Maintenance 4 Omega Lens-cs Sampling Cone Extraction Lens-Omega Lens Assembly O-ring Omega Bias Lens-cs Extraction Lens 2 Extraction Lens 1 Skimmer Base Skimmer Cone Figure 79 Sampling Cone, Skimmer Cone and Extraction Lens-Omega Lens Assembly (7500cs) 2 Remove the Extraction Lens- Omega Lens assembly. Using an Allen wrench, loosen the 3 screws securing the Skimmer Base. Wear laboratory gloves while removing the lens assembly with the Skimmer Base. Place the component on a clean surface.
4 Maintenance Skimmer Base screws (3) Through Hole Skimmer Base Spacer (lipped) Spacer (lipped) Spacer (lipped) Spacer (lipped) Spacer (no lip) Lens Screws (2) Extraction Lens 1 Extraction Lens 2 Omega Lens-ce Omega Bias Guide Omega Bias-ce Omega Bias Guide screw Figure 80 4-100 Expanded View of the Extraction Lens-Omega Lens Assembly (7500cx) Agilent 7500 Series ICP-MS Hardware Manual
Maintenance 4 Skimmer Base screws (3) Through Hole Spacer (lipped) Spacer (lipped) Spacer (lipped) Omega Lens-cs Spacer (no lip) Spacer (lipped) Extraction Lens 1 Extraction Lens 2 Omega Bias Guide Lens Screws (2) Omega Bias Guide Omega Bias Guide Screw Figure 81 Omega Bias-cs Expanded View of the Extraction Lens-Omega Lens Assembly (7500cs) Agilent 7500 Series ICP-MS Hardware Manual 4-101
4 Maintenance Removing the Reaction Cell Assembly The Reaction cell assembly is located inside the vacuum chamber, behind the gate valve assembly. (Figure 82) Reaction Cell screw Reaction Cell Assembly Figure 82 CAUTION Reaction Cell Assembly Disassemble the Reaction cell in an area free of contamination. The following procedure describes how to remove the Reaction cell assembly: 1 Set the Agilent 7500 to shutdown mode and switch off the power.
Maintenance 4 2 Equalize the pressure in the vacuum chamber and remove the chamber cover. Refer to “Working Inside the Vacuum Chamber” on page 4- 94 in this chapter. 3 Remove the tube. Remove the reaction gas tube from the Reaction cell assembly. Reaction Gas Tube Reaction Cell Screw Plate Bias Wire Terminal Screw Reaction Cell Wire Connector Reaction Cell Assembly Plate Bias Wire Figure 83 Reaction Cell as Refitted 4 Remove the connector. Remove the wire connector from the Reaction cell assembly.
4 Maintenance Disassembling the Reaction Cell Assembly Disassemble the Reaction cell assembly after you have removed it from the vacuum chamber. CAUTION Disassemble the Reaction cell assembly in an area free of contamination and while wearing laboratory gloves. 1 Remove the Plate Bias wire. Loosen the 2 Plate Bias wire relay screws from the Cell Exit lens. Remove the 2 Plate Bias wires from the Cell Exit lens (Figure 84).
Maintenance 4 3 Remove the cell assembly screws. Remove the 4 screws located on the bottom side of the Reaction cell assembly to open the Reaction cell. Remove the upper block allowing the Octopole assembly to remain on the lower block.
4 Maintenance 4 Remove the Cell Focus, Cell Entrance Lens, and Spacer. The Cell Focus, Cell Entrance Lens, and spacer are layered together and secured with the Cell Entrance Lens assembly screw. Loosen the Cell Entrance Lens assembly screw to remove the Cell Focus, Cell Entrance Lens, and spacer from the Octopole assembly. CAUTION The Cell Focus, Cell Entrance Lens, QP Focus, Cell Exit Lens and spacer are located on either side of the Octopole.
Maintenance 4 5 Secure the Octopole plate. Secure the Octopole Plate to the location from which you removed the Cell Focus and Cell Entrance Lens. Octpole Octpole Plate Cell Entrance Lens/Cell Exit Lens Screws Figure 87 Securing the Octopole Plate 6 Remove the Cell Exit Lens, QP Focus, and Spacer. The Cell Exit Lens, QP Focus, and spacer are layered together and secured with the Cell Exit Lens assembly screw. Remove the Cell Exit Lens assembly screw to remove all 3 components.
4 Maintenance 7 Secure the Octopole plate. Secure the Octopole plate to the location from which you removed the Cell Exit Lens and QP Focus. Remove the two plate bias relay screws from the Cell Exit Lens. Cell Exit Lens Spacer (Exit Side) QP Focus Octopole Plate Cell Entrance Lens Spacer (Entrance Side) Cell Focus Figure 89 The Octopole with the Cell Entrance Lens and Cell Exit Lens Removed 8 Remove the 2 plate bias relay screws from the cell exit lens.
Maintenance 4 Removing the Plate Bias Lens The Plate Bias Lens is located in the vacuum chamber, between the Reaction cell assembly and the Q- pole. (Figure 90) Plate Bias Lens Plate Bias Lens Screws (2) Cell Exit Guide Figure 90 CAUTION Plate Bias Lens Location (with the Reaction Cell Assembly Removed) Always perform these maintenance in a contamination-free area.
4 Maintenance It is necessary to remove the Reaction cell assembly before removing the Plate Bias Lens. The following procedure describes how to remove the Plate Bias Lens. 1 Remove the Reaction cell assembly. For information on removing the Reaction cell assembly, refer to the previous procedure entitled “Removing the Reaction Cell Assembly” on page 4- 102. 2 Remove the Plate Bias Lens. Loosen the 2 screws securing the Plate Bias Lens and remove the Cell Exit Guide and Plate Bias Lens.
Maintenance 4 Cleaning the Extraction and Omega Lenses It is possible to clean the Extraction Lens, Omega Lens- ce (- cs), and Omega Bias- ce (- cs) separately, but it is more efficient to clean them together. There is normally no need to clean the spacers and screws. Be careful not to touch the spacers and screws with your bare hands. Perform the following procedure when cleaning the Extraction and Omega Lenses. WA R N I N G Do not clean with methanol or acetone.
4 Maintenance 2 Polish with polishing paper (#1200). 3 Clean the orifice of each lens using an almunia powder slurry. Use a mixture of alumia powder and pure water as a polishing solution. Dip a cotton swab in the polishing solution and clean the inner and outer surfaces of the lenses. Pay particular attention to the holes. 4 Rinse with pure water after cleaning. 5 Ultrasonic the lenses in a 2% detergent solution for 5 minutes after cleaning. 6 Rinse with pure water.
Maintenance 4 Cleaning the Reaction Cell Lenses The parts of the Reaction cell that need to be cleaned are the Cell Entrance, Cell Focus, Exit, QP Focus, and Plate Bias Lens. Remove the O- rings from the Cell Entrance and QP Focus lenses when cleaning. It is possible to clean the lenses separately, but it is more efficient to clean them together. There is normally no need to clean the spacers and screws. Be careful not to touch the spacers and screws with your bare hands.
4 Maintenance CAUTION Do not clean plastic components (spacers) with acetone. The plastic will be damaged or deformed if it comes in contact with acetone. Completely dry all components. If components are connected to the vacuum chamber before they have completely dried, it will take an extraordinarily long time for the chamber to pump down to Standby mode. If the printed circuit board has been removed from the Cell’s upper cover, pay attention to the direction when re-attaching it.
Maintenance 4 Refitting the Plate Bias Lens When refitting lenses in the vacuum chamber, begin with the Plate Bias Lens. If you refit the Reaction cell assembly first, you will not be able to install the Plate Bias Lens. Always wear laboratory gloves when refitting the Plate Bias Lens. The following procedure explains how to refit the lens: 1 Install the Plate Bias Lens and Cell Exit Guide in the vacuum chamber. Install the Plate Bias Lens in the direction illustrated in Figure 91.
4 Maintenance 2 Install the Octopole Assembly. Reassemble the Cell Focus, Cell Entrance Lens, QP Focus, and Cell Exit Lens on both sides of the Octopole assembly in their original order. Reassemble the Cell Entrance Lens together with the Entrance side spacer and Cell Focus. Reassemble the QP Focus together with the Exit side spacer and Cell Exit Lens. (Refer to Figure 89) The dimensions of the Octopole are different on the Entrance and Exit sides, so make sure it is assembled in the correct direction.
Maintenance 4 Octopole Holder Contour Octopole Assembly Octpole Shaft Cell Lower Block A-A' Profile Figure 93 Reaction cell assembly 4 Place the cell upper block on the cell lower block. Confirm that the cell upper block is covering the Octopole assembly and is correctly installed over the cell lower block. 5 Tighten the cell assembly screws. Tighten the 4 cell assembly screws from the bottom side of the cell lower block.
4 Maintenance Cell Upper Block QP Focus Cell Exit Lens Cell Entrance Lens Octopole Assembly Cell Lower Block Cell Focus Cell Assemly Screws (4) Figure 94 4-118 Reaction cell and cell assembly screws Agilent 7500 Series ICP-MS Hardware Manual
Maintenance 4 6 Connect the Plate Bias wires. Connect the 2 Plate Bias wires to the 2 Plate Bias wire relay screws on the Cell Exit Lens.(Refer to Figure 95) Cell Exit Lens Screws (2) Plate Bias Wires (2) Cell Exit Lens Plate Bias Wire Relay Screws (2) Figure 95 Plate Bias Wires 7 Check for electrical continuity. Using an Ohm meter, confirm there is no continuity between the cell lower block (ground) and each electrode on the Reaction cell wire connector.
4 Maintenance Check for no continuity between the 6 electrodes on the Reaction cell wire connector. Reaction Cell Wire Connector Ohmmeter Figure 97 Checking the continuity (connector and individual electrodes) 8 Check the continuity. Using an Ohm meter, confirm that there is continuity between all wire connector electrodes and the Cell Entrance Lens, QP Focus, and Cell Exit Lens. Cell Exit Lens Electrode Conducting through the QP Focus Electrode Conducting through the Cell Exit Lens,Plate Bias Lens.
Maintenance 4 Refitting the Reaction Cell Assembly Wear laboratory gloves when refitting the Reaction cell assembly. The following procedure explains how to refit the Reaction cell assembly. 1 Install the Reaction cell assembly to the instrument. Remove the vacuum chamber cover. Place the Reaction cell assembly in the vacuum chamber as illustrated in Figure 82. When doing this, make sure the Cell Entrance Lens is inserted into the guide located on the back of the gate valve.
4 Maintenance Refitting the Extraction Lens-Omega Lens Assembly Wear laboratory gloves when refitting the Extraction Lens- Omega Lens assembly and refitting it to the instrument. The following procedure explains how to assemble and refit the lens to the instrument. 1 Refit the Extraction Lens- Omega Lens assembly. When refitting the Extraction and Omega Lenses to the Skimmer Base, refer to the figure (7500cx: Figure 100, 7500cs: Figure 101) for the correct location and orientation of the components.
Maintenance 4 Skimmer Base screws (3) Through Hole Spacer (lipped) Spacer (lipped) Spacer (lipped) Omega Lens-cs Spacer (no lip) Spacer (lipped) Extraction Lens 1 Extraction Lens 2 Omega Bias Guide Lens Screws (2) Omega Bias Guide Omega Bias Guide Screw Figure 101 Omega Bias-cs Expanded View of the Extraction Lens-Omega Lens Assembly (7500cs) 2 Using an Ohm meter, check for no continuity between the Skimmer Base (ground), Extraction Lens, and Omega Lenses.
4 Maintenance Changing the Hardware Information There are two types of the Extraction- Omega Lens Assembly, one for the 7500cx and another for the 7500cs. It is necessary to change the hardware information when a different type of Ion Lens is installed. To change the hardware information for the Ion Lens, complete the following steps: 1 Select Maintenance>>Hardware Setting on the ICP- MS Instrument Control window. The Hardware Settings dialog box appears. 2 Confirm the Ion Lens type.
Maintenance 4 3 If the correct ion lens is not shown in the dialog box, click the Change button. The Change Ion Lens Type dialog box appears. Figure 103 Change Ion Lens Type dialog box 4 Select the correct ion lens and then click OK. 5 Exit the MassHunter Workstation (or ChemStation) software. When changing the ion lens, refer to the following section for tuning.
4 Maintenance 3 In the MassHunter Workstation’s (or ChemStation’s) ICP- MS Instrument Control window, select Maintenance>>Octopole. The Octopole Setup dialog box will appear on the screen. Figure 104 Octopole Setup dialog box 4 In the Octopole Setup dialog box, click the Octopole Matching button. The Octopole Setup dialog box will close and the Octopole will begin adjusting. This function will begin automatically.
Maintenance CAUTION 4 Hydrogen gas is explosive. Follow the Hydrogen Safety Guide and use special caution when handling this gas. To open the Reaction Gas Line Maintenance dialog box, complete the following steps: 1 Select Instrument>>Instrument Control from ICP- MS Top. The ICP- MS Instrument Control window appears. 2 Select Maintenance>>Reaction Gas from the ICP- MS Instrument Control window. 3 If a warning message is displayed, check the content and then click OK.
4 Maintenance • Optional Gas: Optional gas flow rate setting. Enter the flow rate value in the text box and click the Enter button. NOTE Optional Gas is available when the optional gas line is installed. H2 gas is optional for the 7500cx. If an H2 gas line is not connected, H2- gas- related items are grayed out and cannot be selected. • Input: Current value of the parameter related to vacuum and gas flow. • Close: Close Reaction Gas Line Maintenance dialog box.
Maintenance 4 Maintaining the Electron Multiplier The detector used in the Agilent 7500 is an Electron Multiplier (EM). The EM converts incident ions into an electric current and amplifies the current so the ion signal can be measured. As the voltage applied to the EM increases, the amplification factor (gain) of the current also increases. The EM outputs electric currents in pulses corresponding to each of the incident ions.
4 Maintenance 3 Vent the analyzer vacuum and remove the vacuum cover. Refer to “Working Inside the Vacuum Chamber” in this chapter. 4 Remove the three screws securing the EM cover and slide the cover away from the EM (Figure 106).
Maintenance Figure 107 4 EM Agilent 7500 Series ICP-MS Hardware Manual 4-131
4 Maintenance 5 Loosen the four screws securing the EM, slide it back and remove the EM. There is no need to remove the screws. (Figure 108) EM Vacuum Chamber Figure 108 EM and Vacuum Chamber 6 Install a new EM and secure with the 4 screws, connect the feedthrough leads. 7 Ensure that the electrical leads are positioned well clear of the surrounding wall and the EM body. This is important to avoid any chance of a short- circuit occurring.
Maintenance 4 Changing the Hardware Information There are two types of detectors, 5184- 1983 (ETP AF222) / G1833- 65420 (ETP AF220) and G1833- 65575 (HPK). When a different type of detector is installed, it is necessary to change the hardware information. Both types of detector have a unique method to optimize the supplied High Voltage. It is necessary to identify which detector is installed, then its optimization method is automatically selected.
4 Maintenance 2 Confirm the Detector Type. This dialog box shows the type of Detector. There are two types of detector, 5184- 1983 (ETP AF222) / G1833- 65420 (ETP AF220) and G1833- 65575 (HPK). In this block, click Change after installation and select the detector you have installed. Figure 109 Hardware Settings dialog box 3 If the right detector is not shown in this dialog box, click Change button. The Change Detector Type dialog box appears.
Maintenance 4 Adjustment Procedure after Replacing the EM After replacing the EM, put the instrument into Analysis mode and adjust the discriminator and EM voltage. To adjust the EM, complete the following steps: 1 Put the instrument into Analysis mode. 2 Set the EM voltage (Analog HV, Pulse HV) to the appropriate value as shown below. • Analog HV: 1800 V • Pulse HV: 900 V Select Instrument>>Tuning from the Top menu to display the tuning window.
4 Maintenance Dead Time Calibration This section describes how to execute the Dead Time Calibration using an erbium (Er) solution. Indium (In) is also available for dead time calibration. To execute Dead Time calibration, follow the next procedure. NOTE Dead time calibration must be performed after replacement of the electron multiplier. 1 Perform a new EM and Adjust Discriminator tune. 2 Prepare the calibration standard solution for Dead Time Calibration. For example, 50ppb Er and 1ppm Er.
Maintenance Figure 112 4 Select Use Dead Time Calibration. 4 Introduce the 50ppb Er solution. Tune the sensitivity to make the count of the major isotope 166Er in the range of 50,000 - 1,000,000 count / 0.1 sec.
4 Maintenance 5 Select Tune >> Dead time calibration. The Select Element for EM Dead time Calibration dialog box is displayed. Figure 113 6 Select Er[164/166] then click OK.
Maintenance 4 7 Check sensitivity for 50ppb Er. Select Check. The sensitivity must be above 50,000 counts. Select OK then Run.. Figure 115 Figure 116 50ppb check.
4 Maintenance Figure 117 50ppb finished. 8 Introduce the 1ppm Er solution. Check sensitivity for 1ppm Er. Select Check. Note the increase in sensitivity with this higher concentration. Select OK then Run..
Maintenance Figure 119 4 1ppm Check.
4 Maintenance 9 Select OK to save the new dead time. Typical Dead Time 30 - 60 nano seconds Figure 120 Calibration complete Figure 121 Troubleshooting No signal • Check that the connections of the feedthrough leads are correct. • Check the feedthrough leads do not short- circuit by touching the surround wall such as the EM cover.
Maintenance 4 Maintaining the Penning Gauge The Penning gauge carries a high voltage as it monitors the analyzer vacuum. Before maintaining the Penning gauge, shut down and unplug the instrument. You need to clean this gauge if there is a sudden fluctuation in the (AN) vacuum meter reading of more than 5x10- 3 Pa while you are monitoring the meter. In this block, the typical change of the meter value is more than ±10%. Spiking signals are another indication of the need to maintain the Penning gauge.
4 Maintenance Removing the Penning Gauge Use a clean dry surface and gloves. To disassemble the Penning gauge, complete the following steps: 1 Shut down the instrument. Refer to Chapter 3, “Startup, Shutdown and Status”. WA R N I N G This procedure can expose you to the high voltages of the Agilent 7500, which can be lethal. Before proceeding, completely shut down the instrument. 2 Open the right hood and vent the analyzer vacuum. Refer to “Working Inside the Vacuum Chamber” in this chapter.
Maintenance Figure 122 4 Penning Gauge (A: Magnet Housing, B: Body Tube) Refitting the Penning Gauge Reassemble the Penning gauge in the reverse order of removal. Use gloves and a clean surface as you complete the following steps: 1 Reconfirm that the O- ring is still in place in the manifold (on the back of the vacuum chamber where the Penning gauge fits). 2 With the flange end of the tube toward the vacuum chamber, slide the tube back into the locking plate from below.
4 Maintenance Cleaning the Penning Gauge Replacing the body tube is recommended in the maintenance of the Penning gauge. However, to clean the anode assembly, cathode tube, cathode plate, and body tube, complete the following steps: 1 Remove the electrode from the body tube Using a flat spanner unscrew and remove the collar. Then, using the circlip pliers, remove the anode assembly, cathode plate, and cathode tube from the body tube (Figure 123 on page 4- 146).
Maintenance 4 2 Clean the anode assembly and the inside of the cathode tube Polish the bar of the anode assembly, the gap between the shield disk and the striker 2, and the inside of the cathode tube with 400 grade polishing paper (Figure 124). Anode Polish Cathode Tube Shield Disk Striker 2 Striker 1 Guard Ring Figure 124 Polish inside Tube Cathode Plate Anode Assembly (left), Cathode Tube and Cathode Plate (right) 3 Wash and rinse each of the parts.
4 Maintenance a Slide the cathode plate, cathode tube, and circlip into the top (flange end) of the body tube. Use circlip pliers to position the circlip. b Insert the O- ring into the bottom of the body tube Wipe the O- ring to remove any lint and insert it into the bottom of the body tube. c Insert the anode assembly into the bottom of the body tube using your fingers. Do not bend the anode as you insert it through the cathode. d Screw the collar into the bottom of the body tube.
Maintenance 4 Locating Tools and Supplies To change the oil and empty the oil mist filter, the following supplies are needed: • Rotary pump oil • Waste oil container, at least 1 liter in size • Oil funnel • Paper towel Changing the Rotary Pump Oil To change the rotary pump oil, complete the following steps: 1 Shut down the instrument. See Chapter 3, “Startup, Shutdown and Status” for directions to turn off the instrument and pump.
4 Maintenance 4 Discard the used oil. Dispose of the used oil using the correct laboratory procedures. 5 Add the new oil. Remove the oil fill cap on top of the pump and insert the funnel. Pour in the oil until the sight glass registers between Minimum and Maximum (about 1 L). Replace the cap. CAUTION Use only Agilent recommended oil for the rotary pump. 6 Tighten any loose hose connections. 7 Switch the breaker down to the I side (up) to restore rotary pump power.
Maintenance 4 1 Put the Agilent 7500 into Shutdown mode. Refer to Chapter 3, “Startup, Shutdown and Status” for details. 2 Switch off the two breakers labeled “ROTARY PUMP” on the rear of the instrument. (Switch the breaker down to the ‘O’ side.) 3 Remove the four screws securing the upper body to the lower body and remove the upper body. 4 Remove the filter elements. Discard the used filters according to correct laboratory procedures. 5 Wipe the oil from the inside of the block using a paper towel.
4 Maintenance Maintaining the Water Strainer A strainer is attached to the fitting connector in order for the cooling water chiller to provide clean cooling water. Prolonged strainer use results in clogging and water stains. Remove and inspect the strainer annually, cleaning when necessary.
Maintenance 4 To perform the basic maintenance test, complete the following steps: 1 If completely shut down, restart the instrument. See Chapter 3, “Startup, Shutdown and Status” in this manual. 2 Check the status of the instrument meters. See Chapter 3, “Startup, Shutdown and Status” in this manual. 3 Change the instrument to Analysis mode. See Chapter 3, “Startup, Shutdown and Status” in this manual. 4 Tune the instrument.
4 Maintenance 4-154 Agilent 7500 Series ICP-MS Hardware Manual
Agilent 7500 Series ICP-MS Hardware Manual 5 Troubleshooting Viewing and Clearing the Error Log 5-2 Error Messages 5-3 Alarm Messages 5-45 Items to Be Checked in Case of Low Sensitivity 5-51 Items to Be Checked in Standby Mode 5-51 Items to Be Checked in Analysis Mode 5-52 This chapter describes how to check the error log and the error log’s contents, in order to help you resolve Agilent 7500 MassHunter Workstation (or ChemStation) problems efficiently and effectively.
5 Troubleshooting Viewing and Clearing the Error Log The error log is useful when working to resolve a problem with the Agilent 7500. See the following section for a list of the MassHunter Workstation (and ChemStation) error messages and appropriate responses. Use the following procedures to view and clear the error log. NOTE The error log can become very large and so it must be cleared periodically or it will take up a large amount of disk space.
Troubleshooting 5 Error Messages The following messages can appear in the MassHunter Workstation (and ChemStation) green message bar when you operate the Agilent 7500. When an error message is displayed, the instrument runs a safety sequence. NOTE An * (asterisk) indicates that error number has multiple messages and contents. Please check the error message and error number to properly identify the problem.
5 Troubleshooting • The cooling water is insufficient (possibility of a water leak). • The tubing in the ICP- MS is clogged and the electromagnetic valve is defective. • Either the flow rate sensor or the System I/O board is out of order. 1006* Execution Error: Cooling water (RF/WC/IF) flow rate is too low. The designated command cannot be executed because the cooling water flow rate (RF/WC/IF) is below the limit. Check cooling water flow rate (RF/WC/IF). The following causes are inferred.
Troubleshooting 5 • The vacuum tubing has failed (the tubing is off, or a leak is caused by an incomplete seal such as a pin hole or a defective O- ring.) • There is a fault in the backing Pirani gauge or the System I/O Board. 1009* Execution Error: Vacuum pressure (IF/BK) is too high. The turbomolecular pump cannot work because the vacuum pressure (IF/BK) exceeds the limit (When the instrument is changing from the Shutdown Mode to the Standby Mode). Check the vacuum pressure (IF/BK).
5 Troubleshooting • The vacuum tubing has failed (the tubing is off, or a leak is caused by an incomplete seal such as a pin hole or a defective O- ring.) • A drop of water was introduced into the vacuum chamber. • There is a fault in the Pirani gauge (IF/BK) or the System I/O Board. 1011 Execution Error: Can not execute because the Gate valve is open. Attempted to execute a command that cannot be executed when the gate valve is open. The gate valve is open now.
Troubleshooting 5 • The vacuum tubing has failed (the tubing is off, or a leak is caused by an incomplete seal such as a pin hole or a defective O- ring.) • There is a fault in the backing Pirani gauge or the System I/O Board. 1016* Execution Error: Vacuum pressure (IF/BK) is too high to turn on the Penning gauge (AN). The Penning gauge cannot work because the vacuum pressure (IF/BK) exceeds the limit. (When the instrument is changing from the Shutdown Mode to the Standby Mode).
5 Troubleshooting The following causes are inferred. • Either the large cover or the small cover is opened, or S24V is not supplied for other reason- - - check the voltage of the S24V. • The lenses or the lens and the chamber are touching each other. • There is a fault in the HV driver board. 1021 Execution Error: Turbos slow speed must be done in Standby mode and Vacuum pressure (AN) is low.
Troubleshooting 1026 5 Execution Error: Can not turn on 24V power supply because of RF cable disconnection. The designated command cannot be executed because the cable in the RF generator is not connected or damaged connector. It is possible that the plasma RF generator is faulty. 1027 Execution Error: Can not ignite plasma because of RF cable disconnection. The designated command cannot be executed because the cable in the RF generator is not connected or damaged connector.
5 Troubleshooting 1092 Error: Flash ROM write error. Flash ROM error occurred during writing. The following causes are inferred: • Flash ROM is damaged • Flash ROM is not installed • Flash ROM erase is not possible • Flash ROM cannot write to the firmware (Contact an Agilent Technologies engineer) 1099 Execution Error: Instrument is busy- Between Transition Modes. Attempted to execute a command that cannot be executed during mode transition. The mode is under transition now.
Troubleshooting 5 1102* Error: Vacuum (BK) time out, vacuum too high to switch on Penning gauge (AN). The Penning gauge cannot be turned on because the vacuum pressure (BK) was not managed below the limit within the prescribed time (When the instrument is changing from Shutdown Mode to Standby Mode). Check the backing line pressure. The following causes are inferred. • The vent valve is not closed or the seal is incomplete. • The cover of the vacuum chamber is not closed or the seal is incomplete.
5 Troubleshooting Check the backing line pressure. The following causes are inferred. • The vent valve is not closed or the seal is incomplete. • The cover of the vacuum chamber is not closed or the seal is incomplete. • The power of the rotary pump is not connected or the breaker is OFF. • The rotary pump oil level is low or the oil is dirty. • There is a leak in the gate valve.
Troubleshooting 5 1104* Error: Vacuum pressure (IF/BK) is too high to keep the Penning gauge (AN) ON. The Penning gauge cannot be turned ON because the vacuum pressure (IF/BK) exceeds the limit or the Penning gauge was turned OFF because the vacuum pressure rose abnormally (When the instrument is changing from Shutdown Mode to Standby Mode). Check the vacuum pressure (IF/BK). The following causes are inferred. • The vent valve is not closed or the seal is incomplete.
5 Troubleshooting Check the vacuum pressure (IF/BK). The following causes are inferred. • The vent valve is not closed or the seal is incomplete. • The cover of the vacuum chamber is not closed or the seal is incomplete. • The power of the rotary pump is not connected or the breaker is OFF. • The rotary pump oil level is low or the oil is dirty. • There is a leak in the gate valve.
Troubleshooting 5 • The vacuum tubing has failed (the tubing is off, or a leak is caused by an incomplete seal such as a pin hole or a defective O- ring). • There is a fault in the Pirani gauge (IF/BK) or the System I/O Board. 1112* Error: Pirani gauge (BK) malfunction (Open). There is a fault in the backing Pirani gauge or the System I/O Board (In Analysis Mode). 1112* Error: Pirani gauge (IF/BK) malfunction (Open).
5 Troubleshooting 1114 Error: Pirani gauge (BK) malfunction (Open). There is a fault in the backing of the Pirani gauge or the System I/O Board (When the instrument is changing from Analysis Mode to Standby Mode). 1115* Error: Vacuum pressure (BK) is too high to keep the Penning gauge (AN) ON.
Troubleshooting 1117 5 Error: Pirani gauge (IF) malfunction (Open). There is a fault in the interface of the Pirani gauge or the System I/O Board (When the instrument is changing from Standby Mode to Analysis Mode). 1118* Error: Vacuum pressure (IF) time out vacuum too high to open the gate valve. The gate valve cannot be opened because the vacuum pressure (IF) was not managed lower than the limit within the prescribed time (When the instrument is changing from Standby Mode to Analysis Mode).
5 Troubleshooting • • • • The plasma is too far from the sampling cone. The power of the rotary pump is not connected or the breaker is OFF. The rotary pump oil level is low or the oil is dirty. The vacuum tubing has failed (the tubing is off, or a leak is caused by an incomplete seal such as a pin hole or a defective O- ring). • A drop of water was introduced into the vacuum chamber. 1119* Error: Vacuum pressure (IF/BK) is too high to open gate valve.
Troubleshooting 5 • The vacuum tubing has failed (the tubing is off, or a leak is caused by an incomplete seal such as a pin hole or a defective O- ring). • A drop of water was introduced into the vacuum chamber. 1121* Error: Pirani gauge (BK) malfunction (Open). There is a fault in the interface of the Pirani gauge or in the Pirani gauge control circuit (In Analysis Mode). 1121* Error: Pirani gauge (IF/BK) malfunction (Open).
5 Troubleshooting Check the pressure of the analyzer chamber and the interface line. The following causes are inferred. • The orifice of the sampling cone is too big. • The seal the sampling cone is incomplete (Defective O- ring). • The plasma is too far from the sampling cone. • The diameter of the hole in the skimmer cone is too big. • The installation of the skimmer cone and skimmer base is incomplete. • The installation of the ion lenses is incomplete.
Troubleshooting 5 Check the pressure of the analyzer chamber and the interface line. The following causes are inferred. • The diameter of the hole in the sampling cone is too big. • The seal of the sampling cone is incomplete (Defective O- ring). • The plasma is too far from the sampling cone. • The diameter of the hole in the skimmer cone is too big. • Installation of the skimmer cone and skimmer base is incomplete. • Installation of the ion lenses is incomplete.
5 Troubleshooting Check the number of revolutions and the current of the turbomolecular pump (A), vacuum pressure (AN), vacuum pressure (BK), and S75 power voltage. The following causes are inferred. • A rise in the vacuum pressure. • The connector of the turbomolecular pump (A) came off. • Faulty turbomolecular pump power (S75). • Faulty turbomolecular pump (A) or turbomolecular pump controller (A). • There is a fault in the System I/O Board. 1133* Error: Turbo pump not at desired speed.
Troubleshooting 5 Check the number of revolutions and the current of the turbomolecular pump (I), vacuum pressure (IF), vacuum pressure (BK) and S75 power voltage. The following causes are inferred. • A rise of vacuum pressure. • The connector of the turbomolecular pump (I) came off. • Faulty turbomolecular pump power (S75). • Faulty turbomolecular pump (I) or turbomolecular pump controller (I). • There is a fault in the System I/O Board. 1137 Error: Turbo Pump (A) not at desired speed.
5 Troubleshooting 1139* Error: Turbo Pump not at desired speed. The number of revolutions of the turbomolecular pump went below the limit (In Standby Mode). Check the number of revolutions and the current of the turbomolecular pump, vacuum pressure (AN), vacuum pressure (IF/BK), and S75 power voltage. The following causes are inferred. • A rise in the vacuum pressure. • The connector of the turbomolecular pump came off. • Faulty turbomolecular pump power (S75).
Troubleshooting 5 Check the number of revolutions and the current of the turbomolecular pump (A), vacuum pressure (AN), vacuum pressure (BK), and S75 power voltage. The following causes are inferred. • A rise in the vacuum pressure. • The connector of the turbomolecular pump (A) came off. • Faulty turbomolecular pump power (S75). • Faulty turbomolecular pump (A) or turbomolecular pump controller (A). • There is a fault in the System I/O Board. 1143* Error: Turbo pump not at desired speed.
5 Troubleshooting • • • • 1147 The connector of the turbomolecular pump (A) came off. Faulty turbomolecular pump power (S75). Faulty turbomolecular pump (A) or turbomolecular pump controller (A). There is a fault in the System I/O Board. Error: Gate valve did not close when Plasma off. The gate valve does not close when plasma is extinguished. Check the operation of the gate valve. The following causes are inferred. • Faulty gate valve.
Troubleshooting 1150 5 Error: Penning gauge (AN) fails to strike. The Penning gauge cannot strike. Check the pressure of the analyzer chamber. The following causes are inferred. • The Penning gauge electrode is dirty. • Faulty Penning gauge. • Fault of the System I/O Board. 1151* Error: Turbo Pump (A, I) not at desired speed during penning gauge turn ON. When making a retry of the Penning gauge, the number of revolutions of the turbomolecular pump (A/I) was not within the prescribed range.
5 Troubleshooting 1200 Error: Shunt capacitor time out, did not reach desired value. The Shunt capacitor was not controlled properly. Setting could not be done within the prescribed time. Check the operation of the Shunt capacitor. The following causes are inferred. • Defective drive mechanism of the Shunt capacitor, such as loosened screws. • Defective potentiometer to detect the position of the Shunt capacitor. • Fault in the wiring of the Shunt capacitor drive motor or the potentiometer.
Troubleshooting 5 • The Plasma RF cable came off or the cables are defective. • Malfunction of the Shunt condenser and Series condenser (Faulty XYZMN Board is also probable). • The power cable to the plasma RF generator comes off. • Faulty plasma RF generator. 1204 Error: Turbo is not slowing at Ar purge. During the argon purge, the number of revolutions of the turbomolecular pump did not go below the limit within the prescribed time.
5 Troubleshooting After the purge, if the number of revolutions of the turbomolecular pump does not go down, the following causes are inferred. • Faulty turbo pump controller. • Faulty System I/O Board. 1208* Error: Interface Pressure remained high following gate valve opening. After opening the gate valve, the vacuum pressure (IF) did not go below the limit (When the instrument is changing from Standby Mode to Analysis Mode).
Troubleshooting 5 • Fault in the wiring of the Shunt capacitor drive motor or the potentiometer. • Faulty MNBXYZ Board. 1210 Error: RF amp FET drain current is too high. The output of the FET drain current of the plasma RF amps exceed the limit. Check the plasma RF amp output FET drain current, the plasma RF forward power, the reflected power, the argon gas line pressure, and flow rate.
5 Troubleshooting 1211* Error: DC/DC converter (24/12V) of RF generator malfunction. The DC/DC converter of the plasma RF generator does not work properly. Check the output voltage of the DC/DC converter (Local 12V) of the plasma RF generator. It is possible that the plasma RF driver board is faulty. 1212 Error: RF48V power voltage is too high. The voltage of RF 48V exceeds the limit. Check the voltage of RF 48V power supply. RF 48V is supplied with S24V. The following causes are inferred.
Troubleshooting 5 Check the output of the FET drain voltage of the plasma RF amp, plasma RF forward power, reflected power, argon gas line pressure, and flow rate. The following causes are inferred. • Poor connection of the RF amp directional coupler (connector comes off) • The installation of the torch, bonnet, and shield plate is faulty. • The Argon gas is not supplied or there is a leak in the gas line. • The air or N2 is mixed with argon gas.
5 Troubleshooting 1217 Error: Matching box fan failure. The number of revolutions of the matching box cooling fan went below the limit. Check the number of revolutions of the matching box cooling fan. The cooling fan, cooling fan wiring or MNBXY board is abnormal. 1218 Error: Plasma was shut off. (Plasma RF Monitor). The plasma has extinguished (In Analysis mode or during maintenance). Check the argon gas line pressure and flow rate. The following causes are inferred.
Troubleshooting 5 • The air is mixed with argon gas. • The Plasma RF cable came off or the cables are defective. • Malfunction of the Shunt condenser and Series condenser (A faulty XYZMN Board is also probable). • Power cable to the plasma RF generator came off. • Faulty plasma RF generator 1220 Error: Plasma was shut off during Analysis. (Vac) The plasma has extinguished (In Analysis Mode or during Maintenance). Check the argon gas line pressure and flow rate. The following causes are inferred.
5 Troubleshooting 1300 Error: QP fan malfunction The number of revolutions of the QP driver unit cooling fan went below the limit. Check the number of the revolutions of the QP driver unit cooling fan. Either the cooling fan, cooling fan wiring, or the QP driver board is abnormal. 1301 Error: QP control (Feedback circuit) malfunction. The V voltage of the QP cannot be controlled. Check the V voltage of the QP and QP- RF forward power, reflected RF power. The following causes are inferred.
Troubleshooting 5 • QP rod, or QP- related wiring (including the vacuum chamber) causes a short in other metallic parts. • Either the QP power board or the QP driver board is faulty. 1305 Error: - 600V power supply voltage is too high. The voltage of the DC/DC converter (- 600 V) of the QP driver unit exceeds the limit. Check the QP driver - 600 V power voltage. Either the QP power board or QP driver board may be faulty. 1306 Error: QP amp temperature is too high.
5 Troubleshooting • • • • • • The power of the cooling water chiller is OFF. Cooling water valve is closed. Cooling water is insufficient (possibility of a water leak). Cooling pipes are clogged or leaked. Cooling water strainer is clogged. Cooling chiller is faulty. 1400* Error: Cooling water (RF/WC/IF) flow rate is too low. The flow rate of the cooling water (RF/WC/IF) is below the limit. Check the flow rate of the cooling water. The following causes are inferred.
Troubleshooting 5 The torch position may not be correct. Initialize the torch box. If Time out occurs repeatedly, the XYZMN board may be faulty. 1416 Error: Torch position X- axis initialization failed. Initializing the X- axis has failed. Now, the torch position is not correct. Check if the limit switch of the X- axis works properly and if there is any cause for malfunction, such as something stuck in a direction of the X- axis origin point. If any cause is found, get rid of it to initialize again.
5 Troubleshooting Check the output voltage of the 24V power supply. The following causes are inferred. • The main power supply is faulty. • The board in the instrument is faulty. • The wiring is abnormal. 1434 Error: QP 48V power supply malfunction. The QP 48V power supply malfunction. Check the output voltage of the QP 48V power supply. The following causes are inferred. • The main power supply is faulty. • The System I/O board or QP AMP unit is faulty. • The wiring is abnormal.
Troubleshooting 5 1440* Error: Cooling water (RF/WC/IF) flow rate is too low. Spray chamber temperature control turned OFF. The flow rate of the cooling water (RF/WC/IF) is below the limit, and the cooling of the spray chamber is stopped. Check the flow rate of the cooling water. The following causes are inferred. • The power of the cooling water chiller is not switched on. • The cooling water valve is closed. • The cooling water is insufficient (possibility of a water leak).
5 Troubleshooting • • • • 1446 Faulty argon gas electromagnetic valve (Connector came off). Faulty mass flow controller connector. Faulty mass flow controller. Faulty Introduction board. Error: Aux gas flow rate is too low. The Auxiliary gas flow rate is below the limit. Check the flow rate of the auxiliary gas. Also check the pressure of the argon tank. The following causes are inferred. • The pressure of the argon tank went down.
Troubleshooting 5 Check the pressure of argon gas tank. The following causes are inferred. • Faulty mass flow controller (Connector came off or internal fault). • Faulty Introduction board. 1453 Error: Carrier gas MFC zero adjustment malfunction. The Mass flow controller has failed in zero adjustment. Check the pressure of argon gas tank. The following causes are inferred. • Faulty mass flow controller (Connector came off or internal fault). • Faulty Introduction board.
5 Troubleshooting 1521 Error: System I/O Board controller communication Error. The communication between the boards cannot be performed properly. Check that all the communication lines and the power line are connected properly. Faulty communication lines or Introduction board is inferred as the cause. 1522 Error: QP Driver Board controller communication Error. The communication between the boards cannot be performed properly.
Troubleshooting 5 Alarm Messages The following alarm messages can appear in the MassHunter Workstation (and ChemStation) green message bar when you operate the Agilent 7500. When an alarm message is displayed, the instrument runs a safety sequence. 2150* Warning: Interface Vacuum is too low. The interface line pressure is below the limit (In Analysis Mode). Check the interface line pressure. The following causes are inferred. • The orifice of the sampling cone is too small or clogged.
5 Troubleshooting • • • • • • • • • • • • 2153 The orifice of the sampling cone is too big. The seal of the sampling cone is incomplete (Defective O- ring). The plasma is too far from the sampling cone. The power of the rotary pump is not connected or the breaker is OFF. The rotary pump oil level is low or the oil is dirty. The vacuum tubing has failed (the tubing is off, or a leak is caused by an incomplete seal such as a pin hole or a defective O- ring).
Troubleshooting 5 • Cooling chiller is faulty. 2402 Warning: Cooling water (RF) flow rate is low. The flow rate of the cooling water (RF) is below the limit. Check the flow rate of the cooling water. The following causes are inferred. • The power of the cooling water chiller is OFF. • Cooling water valve is closed. • Cooling water is insufficient (possibility of a water leak). • Cooling pipes are clogged or leaked. • Cooling water strainer is clogged. • Cooling chiller is faulty.
5 Troubleshooting 2404 Warning: Cooling water temperature is low. The temperature of the cooling water is below the limit. Check the temperature of the cooling water. When the setting of the cooling chiller is not correct or faulty, this error may be generated. 2405 Warning: RF Driver voltage is high. The voltage of RF Driver exceeds the limit. It is possible that the output power of the RF generator is not controlled properly. The following causes are inferred.
Troubleshooting • • • • 2415 5 Faulty argon gas electromagnetic valve (Connector came off). Faulty mass flow controller connector. Faulty mass flow controller. Faulty Introduction board. Warning: Makeup gas flow rate is low. The flow rate of the makeup gas is below the limit. Check the flow rate of the makeup gas. Check the pressure of the argon tank. The following causes are inferred. • The pressure of the argon tank fell. • Gas line fault such as clogging or coming off.
5 Troubleshooting 2606 Warning: Z- axis Torch position is outside the warning limit. The Z- axis torch position moved beyond the warning limit. 2607 Warning: Y- Axis movement disabled due to partially closed top cover. The torch box tried to move, but failed because the small cover was not opened fully. Try it again after opening the small cover fully. There may be a fault in the small cover Full Open Sensor or a fault in the System I/O board. 2608 Warning: Torch position initialization failed.
Troubleshooting 3004 5 Power Failure occurred. After the power was switched OFF, it was switched ON again. Items to Be Checked in Case of Low Sensitivity If the sensitivity is low, conduct the troubleshooting described in the following “Items to Be Checked in Standby Mode” and “Items to Be Checked in Analysis Mode” sections. If the described procedure does not restore the sensitivity, contact our Customer Contact Center.
5 Troubleshooting Items to Be Checked in Analysis Mode • Check to make sure that the torch is positioned correctly. Using Autotune, adjust the torch vertical/horizontal position • Check to make sure that the mass axis is adjusted correctly. Using Autotune, adjust the Resolution/Axis. • Execute the EM voltage adjustment. Using the Autotune, adjust the EM/discriminator. • Check to make sure that the lens is responding. Check to make sure that the signal changes when the lens voltage is varied.
Agilent 7500 Series ICP-MS Hardware Manual 6 Technical Information Peristaltic Pump and Tubing 6-2 Nebulizer 6-4 Nebulizer Endcap 6-8 Spray Chamber 6-8 ICP Torch 6-9 Interface 6-10 Ion Lenses - Principles of Operation 6-11 Q-pole 6-19 Electron Multiplier (EM) 6-21 APG remote interface 6-23 In this chapter the hardware components of the Agilent 7500 ICP- MS are reviewed, and some descriptions of the theory for operation are included.
6 Technical Information Peristaltic Pump and Tubing The standard peristaltic pump of the Agilent 7500 has three channels to set tubing for the sample solution, internal standard solution, and the spray chamber drain. There are three types of peristaltic pump tubing: • Tygon for sample uptake (white/black, 1.02 mm i.d.) • PharMed for the drain (yellow/blue, 1.524 mm i.d.) • Tygon for the internal standard (orange/red, 0.19 mm i.d.) The colors refer to the peristaltic pump head- stops bonded to the tubing.
Technical Information 6 When the ASX500 Autosampler is used, it takes about 25 seconds for the sample exchange and 15 - 30 seconds for stabilizing the signal. Use 30 seconds on fast pump followed by 20 - 40 seconds stabilization time when the ASX500 is used. The inner diameter of the sample transfer tube (Teflon) is 0.5 mm. A tube smaller than 0.5 mm i.d. can cause the generation of bubbles in samples. This problem may occur due to highly pressurized tap water that contains gases (drinking water samples).
6 Technical Information sample uptake rate to vary, when sample viscosity and sample head volume above the level of the sample aspiration tube change and it can only be used when the sample matrix is similar to that of the standard solution.
Technical Information 6 pressure has to be 500 to 600 kPa (72 to 87 psi), giving about 1.2 L/min carrier gas flow. A 1.0 L/min carrier gas flow rate is recommended and the make- up gas has to be added to the carrier gas to achieve optimal conditions. The recommended sample uptake rate is about 0.4 mL/min, which requires a 0.1 rps peristaltic pump speed.
6 Technical Information Another possible problem is leakage of the Ar gas line and sample line; if the O- rings for the sample tube are not tightened enough, air leaks will occur (Figure 127). This will often be indicated by a higher signal for N, N2 and ArN at m/z 14, 28 and 54, respectively, higher sensitivity for lighter masses and lower sensitivity for heavier masses.
Technical Information 6 PFA Concentric Nebulizer The nebulizer is made of fluorocarbon resin (PFA) and the sample is introduced by self- aspiration. The PFA concentric nebulizer can be used in the same way as the concentric nebulizer and, since it is made of fluorocarbon resin, it can be used for various types of samples such as strong acid, strong base and organic solvent. However, when such samples are introduced, please use the Inert Sample Introduction Kit.
6 Technical Information Nebulizer Endcap Each nebulizer has a dedicated endcap made of Teflon. Except for the CF, the nebulizer can be removed from the endcap. The make- up gas is introduced into the spray chamber through the endcap giving a tangential flow around the nebulizer, except for the CF. Spray Chamber There are several types of spray chambers for ICP- MS. The most commonly used type is the Scott double pass spray chamber, which is employed in the Agilent 7500.
Technical Information 6 solvents attack PP. Since PP is a plastic type material, wetability is not as good as for the QZ and PG. When a PP spray chamber is not in use, it must be kept in an acid bath to maintain wetability. A 5%(v/v) HNO3 bath is recommended. Teflon (PFA) This PFA spray chamber is the standard spray chamber for the inert sample introduction kit, and is used when aspirating hydrofluoric acid.
6 Technical Information Interface Ions in the plasma are extracted into the vacuum chamber through a sampling cone and a skimmer cone. The orifice size of the sampling cone is φ1.0 mm and that of the skimmer cone is φ0.4 mm. There are two types of material used, nickel (Ni) and platinum (Pt). The base material of the sampling cone is Cu and the tip of the cone is Ni. The skimmer cone is all Ni. Pt has to be used for HF solutions and higher concentration of acids.
Technical Information 6 Ion Lenses - Principles of Operation There are three ion lens main components: Extraction lens, Einzel lens and Omega lens. To understand the mechanism of the ion lens, consider equipotential lines of an electrical field (Figure 128). When the electrical field is in parallel and at A volts above the ground level, a positive ion is accelerated as a function of voltage. The Einzel lens consists of three circular- hole lenses, which create the electrical field, see Figure 128.
6 Technical Information capacitive coupling between the plasma and the RF coil, which creates a potential in the plasma (Figure 129). The potential in the plasma is oscillating at the radio frequency of the plasma.
Technical Information 6 Now, consider the inside of the plasma. Since the plasma temperature is high, about 7,000 K under the normal operating conditions, positive ions and electrons exist in the plasma. The number of positive ions and electrons is the same, so, the plasma is electrically neutral. Since the interface is cooled by water, the plasma temperature decreases drastically when the plasma comes close to the interface.
6 Technical Information such as the position of the mach disc, that are affected by the plasma temperature; a lighter mass penetrates through the skimmer cone easier than a heavier mass. Ion Lens Setting Y T1 Sensitivity Li Low Figure 131 Ion Energy High Distribution of Ion Energy Extraction Lens This lens assembly is placed just behind the skimmer cone and mounted on the skimmer base. Its purpose is to extract ions passed through the skimmer cone and to accelerate them to the Einzel lens.
Technical Information 6 Einzel Lens The purpose of this lens assembly is to focus the ions that are accelerated by the extraction lenses. The Einzel lens consists of three lens plates. The same voltage is applied to the first and the third lens plates (E1 and E3) to get the same potential at the entrance and exit of the lens, - 100V, it should not normally be adjusted during tuning. Changing the voltage of the middle lens, the Einzel 2 lens, affects the focal point of the ions.
6 Technical Information Omega (-) Omega (+) Plate Bias + - - + Q-Pole M+ : Photon : Ion Figure 132 Pre-Filter Omega Bias QP Focus Schematic Diagram of Omega Lens The ions then pass through the QP focus and the Plate bias. The purpose of these lenses is to decelerate ion speed and to focus the ions. The QP focus and the Plate bias are operated at zero or slightly positive voltage.
Technical Information 6 Octopole Reaction System Reaction Gas Quandrupole Detector Octopole Reaction Cell Extraction-Omega Lens Figure 133 Off-axis Ion Lens + Octopole Reaction Cell The Octopole Reaction System (ORS) is an octopole ion guide contained within a stainless steel vessel and pressurized with a gas, most often H2 or He. The ORS is positioned between the ion lens assembly and the quadrupole mass filter.
6 Technical Information Why the octopole ion guide? The octopole ion guide is driven by a voltage of fixed amplitude and frequency in order to assure stable signals. The frequency of 10 MHz brings about wiggle- less motion of ion near the flat bottom of the effective potential well, which is difficult to achieve with lower order multipoles or low- frequency voltage2).
Technical Information 6 Gas Flow Tuning Flow rates of the reaction gases are set in the tuning window of Agilent’s MassHunter Workstation (or ChemStation) Software. Due to the ‘MultiTune’ capability of MassHunter Workstation (or ChemStation), reaction gases can also be automatically switched during the analysis. Q-pole The Q- pole of the Agilent 7500 consists of a pre- filter and a main filter. The inner surface of the Q- pole rods is hyperbolic giving an ideal electrical field inside the Q- pole.
6 Technical Information Max.
Technical Information 6 The scan line of a Q- pole is represented in Figure 135. Lower voltages of U and V select lighter masses while higher voltages select heavier masses. Resolution can be expressed as follows: Resolutions ∝ f 2L2/V f : Frequency L : Length of Q- Pole V : Speed of Ion So, higher ion speed, shorter Q- pole length or lower frequency results in poorer resolution. When the Q- pole becomes dirty, the peak shape will be poor even if a higher pole bias is applied.
6 Technical Information accumulated by the accumulator. The accumulated value is then converted to pulse counts by the P/A factor (Figure 136). They are generally called dual mode. For adjustment of the dual mode, a P/A factor must be set. When data acquisition starts, the Smart Card and the CPU board automatically select which masses are analyzed by the pulse mode and by the analog mode; the switching level is about 1 x 106 cps.
Technical Information 6 APG remote interface The following functions are available on the Agilent 7500 MassHunter Workstation (or ChemStation) APG remote interface.
6 Technical Information N/A: Not Applicable Pin 3, Start: Request to start run. Start the Data Acquisition. Pin4, Shutdown: When Standard is selected in the Remote Shutdown section of the Miscellaneous dialog box. The Miscellaneous dialog box appears when Setup is clicked in the Miscellaneous area of the ICP- MS Configuration dialog box. Receive: When the instrument is in the Analysis mode and the signal is changed to LOW, the instrument goes to the Standby mode.
Agilent 7500 Series ICP-MS Hardware Manual Appendix Appendix A.
Appendix Appendix A. Organic Solvent Kit Organic Solvent Kit General When analyzing organic solvents, Oxygen must be added in to the carrier gas line to burn the carbon in the organic solvent. This will avoid depositing the carbon on to the interface (Sampling cone / Skimmer cone). If the deposition is allowed to build up the interface cones can clog. A 1.5mm (or 1mm) I.D torch is used for organic solvent samples to maintain good plasma conditions.
Appendix Agilent 7500 Spray Chamber Mass Flow Controller To Torch Make up Gas Carrier Gas Mass Flow Controller Mixture Gas (O2 20%, Ar 80%) Argon Gas CAUTION Option Gas Set the Option Mass Flow tank Pressure at 350kPa.
Appendix WA R N I N G Use 20% Oxygen and 80% Ar gas mixture. There is an increased risk of explosion or fire if higher concentrations of Oxygen are used. If the equipment is used connected to highly concentrated oxygen gas, and the oxygen gas keeps flowing due to the above-mentioned irregularities, dangers arise as detailed below. • Inflammability, explosibility, etc. of oxygen • Since oxygen is an ignitable gas, oxygen does not burn by itself, but it assists the combustion of other substances.
Appendix Replacing the torch and connector 1 Locate and open the torch box. 2 Remove the existing torch and connector. 3 Install the Connectors for Optional Gas Introduction and 1.5mm (or 1mm) I.D. Torch. 4 Insert the Inner Sleeve into the Option gas Line and connect the option gas line to the Connectors for Optional Gas Introduction using the L type Teflon connector. Teflon Tubing CAUTION Inner Sleeve Connect the Teflon tubing to the connector securely.
Appendix O-ring for Nebulizer and Endcap Replace the O- ring for the Nebulizer and End Cap with O- ring's that are resistant to organic solvents. QTY P/N O-ring for Organic Solvent (Nebulizer) 1 G1820-65520 O-ring for Organic Solvent (Endcap) 1 G1820-65518 These O- rings are included in Organic Solvent Kit (G1833- 65424). CAUTION A-6 Neither the standard O-rings nor the solvent resistant O-rings are color coded. Keep the O-rings separately and do not mix them.
Appendix Drain kit for Organic Solvent Organic Solvent drains via the Drain Line from the Spray Chamber. All parts on the drain line should be resistant to organic solvents. Otherwise there could be leakage and it can increase the risk of explosion. WA R N I N G When Introducing the Organic Solvent, use the Organic Solvent Kit. Otherwise there could be leakage and it can increase the risk of explosion.
Appendix The following explains the different points between the standard drain kit and the drain kit for Organic Solvent. (2) Bushing: Material is different. (3) Tubing: Material and ID / OD are different. (4)(6) Connector: OD to connect the Tubing (3) / (7) is different. (7) Tubing: Material and ID / OD are different. (8) Connector of Drain Tank: Material and OD to connect Tubing (7) is different.
Appendix 10 Install the Spray Chamber. 11 Connect tubing between the Drain Tank and Exhaust Port on Backside of 7500. WA R N I N G Confirm there is no leakage at all of the Drain Lines (e,g, outlet of Spray Chamber). If there is leakage, there is increased a risk of explosion. Adjustment of clamp tension for Drain tubing 1 Make sure the drain tubing is not damaged. Replace the drain tubing when it is damaged. 2 Select Instrument >> Instrument Control. 3 Select Maintenance >> Sample Introduction.
Appendix WA R N I N G Confirm that the drainage is flowing. Check that the tube from the drain peristaltic pump to the drain bottle is properly connected. You should see a regular pattern of liquid and air as shown above. WA R N I N G When the spray chamber drain is not pumped properly, excess flammable solvents in the spray chamber may ignite and become explosive. Ensure that the spray chamber drain is being pumped properly during analysis.
Appendix Warning Label Put the warning label from the kit onto the front panel.
Appendix Table 12 Organic solvents having confirmed methods for the Agilent 7500 ICP-MS (Nebulizer; Concentric) Organic solvent Dilution factor *Sample tubing id (mm) Torch injector id (mm) Oxygen % in total carrier & make-up gas iso-propyl alcohol (IPA) direct 0.2 1.5 2% methyl alcohol (Methanol) direct 0.16 1.0 3% ethyl alcohol (Ethanol) direct 0.3 1.5 3% 2,2 aminoethoxy ethanol 1:41% nitric acid 0.5 1.5 None ethyl acetate 1:1 NMP 0.3 1.5 3% buthl acetate 1:1 NMP 0.3 1.
Index Numerics B 3-stage vacuum, 1-19 Babington nebulizer, 3-17, 4-25, 4-29 to 4-33, 4-36 to 4-38, 4-48 to 4-49, 6-3 to 6-4 bench, 1-8 bend mass, 4-126 blank solution(s), 1-17, 6-17 bonnet, 4-59 to 4-65, 5-28, 5-31 to 5-35 bypass valve, 4-127, 5-8 A access, P-2, 1-22, 3-4, 3-13 to 3-14, 4-68 acetone, 2-7, 4-25 to 4-26, 4-31, 4-70, 4-77, 4-87, 4-93, 4-111, 4-112 to 4-114 acid(s), 2-3, 2-5 to 2-6, 4-14 to 4-15, 4-25 to 4-26, 4-30 to 4-32, 4-39, 4-41 to 4-42, 4-45, 4-47 to 4-48, 4-51, 4-55, 4-59, 4-62, 4-6
Index Einzel 3, 4-84 Einzel lens, 1-17, 4-75 to 4-76, 4-77, 4-82 to 4-85, 4-88 to 4-91, 6-11, 6-14, 6-15 electrical outlet, 2-14 electrical power, 1-21, 2-15 electron multiplier (EM), 1-3, 1-16, 1-18, 1-24, 4-4 to 4-5, 4-8, 4-129, 4-136, 6-21 electrostatic charging, 4-18 EM cover, 4-130, 4-132, 4-142 EM voltage, 4-129, 4-135, 5-52, 6-22 Enable Scan, 4-126 end cap, 4-4, 4-14, 4-28 to 4-33, 4-35, 4-36, 4-37 to 4-43, 4-45 to 4-46, 4-48 to 4-50, 6-4 environment, 2-14, 3-14, 4-78, 4-95, 4-129 error log, 4-13, 5
Index nebulizer pump, 4-17 NEMA, 3-2 nitric acid, 4-14 to 4-15, 4-25, 4-30 to 4-32, 4-41 to 4-42, 4-45, 4-48, 4-51, 4-55, 4-59, 4-62, 4-66, 4-71 O odor element, 4-148, 4-150 oil mist (filter), 2-5, 2-9, 4-3, 4-149, 4-150 Omega (-), 6-15 Omega (+), 6-15 Omega Bias, 4-89, 4-90, 4-99, 4-111, 6-15 Omega lens, 1-17, 4-3, 4-75 to 4-76, 4-77, 4-82 to 4-85, 4-88, 4-90 to 4-94, 4-97 to 4-101, 4-111, 4-112, 4-115, 4-122 to 4-124, 6-11, 6-15 to 6-16, 6-19 operator maintenance, 4-2 option(al) gas, 1-7, 1-15, 2-8, 3-1
Index single phase, 2-15 skimmer base, 4-67, 4-72, 4-81, 4-87, 4-90, 4-99, 4-111 to 4-112, 4-122 to 4-123, 5-20, 5-21, 6-10, 6-14 skimmer cone(s), 1-2, 1-16, 1-20, 4-3, 4-66 to 4-67, 4-69 to 4-70, 4-72 to 4-73, 4-80, 4-97 to 4-99, 4-123, 5-20, 5-21, 5-45, 5-51, 6-10, 6-14 solvent(s), 2-6, 4-26, 4-31, 4-49, 4-87, 6-6 to 6-7 spray chamber, 1-2, 1-14 to 1-15, 1-21, 2-7, 3-8, 4-4, 4-14, 4-25 to 4-30, 4-33, 4-38, 4-42 to 4-43, 4-46 to 4-50, 4-52, 4-54, 4-57, 4-60, 4-65, 5-6, 5-40 to 5-42, 6-2, 6-4, 6-8 to 6-9 s
www.agilent.com In This Book The Agilent 7500 Series ICP- MS Hardware Manual provides an instrument overview, safety precautions and procedures for optimization, maintenance and troubleshooting. © Agilent Technologies, Inc. 2008 Printed in USA Rev.
