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Operation

Agilent 5100 and 5110 ICP-OES User’s Guide

53

Restarting the instrument to be ready for analysis again will take
several hours due to the gas purge and polychromator thermal
stabilization time.

NOTE

If the instrument is not going to be in use for a period of time the torch, cone,
snout and torch compartment should be cleaned of any deposits, dirt or residue.
Check the cleanliness of the removable axial window when cone is removed.

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Содержание 5100 ICP-OES

Страница 1: ...Agilent 5100 and 5110 ICP OES User s Guide ...

Страница 2: ... hardware and or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcontract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commerc...

Страница 3: ...as Hazards 10 Electrical Hazards 11 Other Precautions 11 Warning Symbols 13 CE Compliance 14 Electromagnetic Compatibility 15 EN55011 CISPR11 15 ICES NMB 001 16 South Korean Class A EMC declaration 16 2 Introduction 17 Site Preparation Requirements 17 User Documentation 18 Conventions 18 Notes and tips 18 Specifications 19 Temperature control 19 Environmental conditions 19 ...

Страница 4: ...Drain Vessel 23 3 Installation 25 Agilent ICP OES Instrument Overview 26 Instrument Status LED Color Coding 28 Front Power On Off Button 28 ICP Expert Software 29 Connecting ICP Expert software to the ICP OES 30 Performing a Detector and Instrument Calibration 30 Saving and viewing the calibration data 32 Hardware Components Replacement 32 ICP OES torches 33 Torch Assembly and Disassembly 34 Torch...

Страница 5: ...Mist Programmable Temperature Spray Chamber 42 4 Operation 43 Analysis Checklist 43 Turning On the Instrument and Software 44 Turning on the instrument for the first time or from long term shutdown 44 Running the instrument from an idle state 45 Preparing for Analysis 46 Performing a Detector and Instrument Calibration 46 Creating Opening a Worksheet 47 Creating a new worksheet 47 Opening an exist...

Страница 6: ...g off the instrument for long term shutdown 52 5 Maintenance and Troubleshooting 55 Routine 56 Cleaning 58 Torch Cleaning 58 Acid cleaning of the torch for aqueous or acid based samples 59 Rinsing the torch 61 Drying the torch 62 Additional checks after cleaning 63 Troubleshooting 63 Spare Parts 63 Technical Support 64 ...

Страница 7: ...ous materials including corrosive fluids and flammable liquids Careless improper or unskilled use of this spectrometer or chemicals used with it can cause death or serious injury to personnel and or severe damage to equipment and property Only trained personnel should use this instrument The spectrometer incorporates interlocks and covers that are designed to prevent inadvertent contact with any p...

Страница 8: ...gns of corrosion that are likely to inhibit function or safety Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements Plasma The plasma is extremely hot about 10 000 C and radia...

Страница 9: ... torch and torch compartment to cool before carrying out any work in this area or wear heat resistant gloves The plasma system has been carefully designed to operate safely and effectively when using torches and related components that conform to Agilent s design criteria Use of non approved components in the plasma compartment may render the system inoperative and or hazardous It may also invalid...

Страница 10: ...ure or a properly constructed cylinder stand Move cylinders only by securing them to a properly constructed trolley Use only approved regulator and hose connectors refer to the gas supplier s instructions Keep gas cylinders cool and properly labeled All cylinders are fitted with a pressure relief device that will rupture and empty the cylinder if the internal pressure is raised above the safe limi...

Страница 11: ...upting the protective conductor inside or outside the Agilent ICP OES or defeating the power cord ground creates a shock hazard for the operator and can damage the instrument Other Precautions Use of the spectrometer system and accessories may involve materials solvents and solutions which are flammable corrosive toxic or otherwise hazardous Careless improper or unskilled use of such materials sol...

Страница 12: ...uding ensuring adequate ventilation during use and use of lab coats safety goggles gloves and other appropriate forms of personal protection The organic wastes should be disposed of in accordance with local regulatory requirements Air flow to the air intake port of the spectrometer and accessories must be unobstructed Do not block the ventilation grills on the spectrometer and accessories Consult ...

Страница 13: ...icates a warning The meanings of the symbols that may appear alongside warnings in the documentation or on the instrument itself are as follows Broken glass Chemical hazard Electrical shock Extreme cold hazard Eye hazard Fire hazard Heavy weight danger to feet Heavy weight danger to hands Hot surface Noxious gases RF radiation The following symbol may be used on warning labels attached to the inst...

Страница 14: ...Socket for Ethernet LAN cable Socket for Agilent accessory USB cable Indication of correct orientation of gas filter flow direction CE Compliance Your Agilent ICP OES instrument has been designed to comply with the requirements of the Electromagnetic Compatibility EMC Directive and the Machinery Directive MD of the European Union Agilent has confirmed that each product complies with the relevant D...

Страница 15: ...n which there is intentionally generated and or used conductively coupled radio frequency energy which is necessary for the internal functioning of the equipment itself Class A equipment is equipment suitable for use in all establishments other than domestic and those directly connected to a low voltage power supply network which supplies buildings used for domestic purposes This device complies w...

Страница 16: ...ipheral devices are also certified 5 Make sure that appropriate cables are used to connect the device to peripheral equipment 6 Consult your equipment dealer Agilent Technologies or an experienced technician for assistance 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 Canad...

Страница 17: ...our instrument you will have been provided with an Agilent 5100 and 5110 ICP OES Site Preparation Guide which describes the environmental and operating requirements of the ICP OES system You must prepare your laboratory according to these instructions before the ICP OES can be installed You should keep the Site Preparation Guide for future reference for example if you plan to move your instrument ...

Страница 18: ...accessories you ordered A Familiarization DVD that includes information on how to set up methods and run instrument tests some hardware basics and maintenance videos Conventions The following conventions have been used throughout the documentation Menu items menu options and field names for example click Copy from the Edit menu have been typed in bold Bold is also used to signify the buttons appea...

Страница 19: ...cations refer to your Agilent ICP OES Site Preparation Guide Use of power boards or extension cables is not recommended The installation of electrical power supplies must comply with the rules and or regulations imposed by the local authorities responsible for the use of electrical energy in the workplace Avoid using power supplies from a source that may be subject to electrical interference from ...

Страница 20: ...ed with Agilent ICP OES spectrometer systems Agilent recommends the use of liquid gases which are purer more convenient and cheaper per unit volume Table 1 Gas supply requirements Component Gas Plasma nebulizer optics interface purge Argon Polychromator assembly Argon or Nitrogen supplied through optional nitrogen purge kit Gas supply regulator pressure setting may need to be adjusted to ensure th...

Страница 21: ...r maintenance Exhaust system The plasma operates at extremely high temperatures The ICP OES instrument exhaust fumes can be noxious or corrosive The exhaust system should be checked regularly to ensure adequate flow Consult the ICP OES Site Prep Guide for the appropriate flow rates WARNING Hot Surface The external vent may become hot during ICP OES instrument operation and remain hot for some time...

Страница 22: ...ust provide positive air pressure at the instrument inlet of 4 m3 min 141 ft3 min when using the External Inlet Duct Adaptor Kit G8010 68002 The ducting should be corrosion resistant and fire proof Water Chiller System Agilent ICP OES instruments require a source of cooling water Refer to the Site Preparation Guide for compatible water chilling systems and to the documentation provided with the wa...

Страница 23: ...r use with inorganic solvents When using organic solvents different drain tubing that is suitable for the solvent in use will be required A chemically inert container not glass or of a narrow necked style to hold a minimum of 2 liters 4 pints of waste must be provided by the user It should be located underneath the sample compartment or on the right side of the instrument where it is protected by ...

Страница 24: ...Introduction 24 Agilent 5100 and 5110 ICP OES User s Guide This page is intentionally left blank ...

Страница 25: ... Disassembly 34 Accessories 38 The Agilent ICP OES must be installed by an Agilent trained Agilent qualified or Agilent authorized field service engineer You should have completed and returned the form in the Site Preparation Guide stating that you have prepared the laboratory in accordance with the requirements detailed in that manual An Agilent representative will then arrange a suitable install...

Страница 26: ...s window not shown 10 Nebulizer 17 Optics purge filter for argon or nitrogen 4 Snout and radial pre optics window not shown 11 Peristaltic pump 18 Gas supply assembly 5 Induction coil 12 Mains power switch and cable connection 19 Optional AVS 4 AVS 6 or AVS 7 Switching Valve accessory location 6 Torch 13 Front panel power button 20 Drain for liquid overflow 7 Nebulizer and make up gas connections ...

Страница 27: ...nt and the mains power switch is located on the left back side of the instrument Figure 2 Input and output connections on the side of the ICP OES instrument Item Description 1 Accessory and LAN cable connections Agilent accessory connections and Ethernet cable for PC to instrument communication 2 Argon gas inlet Argon gas inlet standard 3 Option gas inlet Option gas 80 Ar 20 O2 mix inlet Optional ...

Страница 28: ...to begin a plasma ignition sequence due to a tripped door or torch handle interlock low gas pressure low water flow or low cooling air flow User intervention is required to resolve the problem An orange pulsing intensifying fading light indicates the instrument is booting up or performing a firmware update A red light indicates an instrument firmware error causing a halt to analysis or restricting...

Страница 29: ...ce engineer will install the ICP Expert software for you during the installation process However you may need to install the software yourself at some later stage for example if you change the PC Instructions are provided There are several installation scenarios Standalone or network Flat File Standalone or network Database for 21 CFR Part 11 installations Upgrading Standalone or Network Database ...

Страница 30: ...ting ICP Expert software to the ICP OES To connect the software and instrument 1 Start the ICP Expert software by double clicking on the desktop icon 2 Click Instrument 3 Click Connect 4 Enter the IP address of the instrument or select an existing instrument 5 Click Connect 6 Click Close Performing a Detector and Instrument Calibration To perform a detector and wavelength calibration 1 Turn on the...

Страница 31: ...nt window of the ICP Expert software click the Status tab and check that under the Polychromator section Boost is selected b If the instrument was turned on from an idle state the wavelength calibration in Steps 7 10 can be performed immediately If the instrument was turned on after more than a few hours of being unpowered the polychromator can take several hours to stabilize the temperature and t...

Страница 32: ...OTE The default save location is Users Username Documents Agilent ICP Expert Exported Results on the drive on which the ICP Expert software is installed Hardware Components Replacement Your ICP OES should be ready to operate after the Agilent field service engineer has installed it However you may need to set up items such as the peristaltic pump nebulizer torch or spray chamber For instructions o...

Страница 33: ... tube material Quartz Quartz Quartz Quartz Quartz Intermediate tube Quartz tulip Quartz tulip Quartz tulip Quartz tulip Quartz tulip Recommended application Most sample types Most sample types Hydrofluoric HF acid digests Samples with high total dissolved solids Semi volatile organic solvents e g ketones kerosene Jet A1 Parameter Radial View Torches Standard torch Demountable torch Inert demountab...

Страница 34: ... torch compartment become warm during instrument operation and remain so for some time after the plasma has been switched off Allow the plasma compartment to cool for at least five minutes before accessing the plasma compartment Allow the torch to cool for two minutes before touching the outer tube or attempting to dismantle the torch WARNING Chemical Hazard Nitric and hydrochloric acids are very ...

Страница 35: ...the torch 1 Position the flat side of the torch securing ring so that it faces the top of the torch Figure 4 Flat side of torch securing ring 2 Slide the torch securing ring approximately 1 3 the way up the torch Figure 5 Torch securing ring on torch 3 Slide the torch into the torch body ...

Страница 36: ...nserted into torch body 4 Position the torch so that the groove on the torch body aligns with the etch mark on the torch Figure 7 Torch alignment 5 Press the torch fully into the torch body and then press down on the torch securing ring Figure 8 Torch inserted into torch body ...

Страница 37: ...ver to loosen the torch securing ring from the torch body if you are unable to do so by hand 1 Insert the screwdriver into the slot between the torch securing ring and the torch body 2 Gently twist the screwdriver to separate the torch securing ring from the torch body Figure 9 Separating the torch securing ring from the torch body 3 Repeat Steps 1 and 2 on the slot on the opposite side 4 Gently s...

Страница 38: ...pler SPS 3 Sample Preparation System Advanced Valve System AVS AVS 4 AVS 6 and AVS 7 switching valves SVS 2 and SVS 2 Switching Valve Systems 5 channel peristaltic pump Air inlet dust filter External inlet duct adapter Vapor generation accessory VGA Multimode sample introduction system MSIS Argon humidifier IsoMist Programmable Temperature Spray Chamber For safety and installation information plea...

Страница 39: ...SPS 3 is compatible with a wide range of commercially available low cost autoclavable sample racks Sample contamination from airborne particles is eliminated and corrosive or toxic fumes are removed during sampling with the optional environmental enclosure Advanced Valve System AVS AVS 4 AVS 6 and AVS 7 For safety information and to prepare the accessory for installation please see the instruction...

Страница 40: ...ation and to prepare the accessory for installation please see the instructions that came with the accessory The SVS 2 and SVS 2 increase sample throughput and decrease turnaround time and operating costs The switching valves are positioned between the nebulizer and the peristaltic pump of the spectrometer Samples are quickly loaded into the sample loop ready for immediate analysis by the ICP OES ...

Страница 41: ... a separate module and can be simply exchanged when switching elements Multimode Sample Introduction System MSIS For safety information and to prepare the MSIS for installation please see the instructions that came with this accessory and the ICP Expert Help The MSIS is used with the ICP OES instrument to provide simultaneous vapor generation of several hydride forming elements enabling determinat...

Страница 42: ...to be beneficial by reducing the build up of salt and other dissolved solids in the sample introduction system By reducing blockages the Argon Humidifier helps to ensure uninterrupted maintenance free operation IsoMist Programmable Temperature Spray Chamber IsoMist utilizes the Peltier effect to provide electrical cooling or heating to the spray chamber The Set Temperature is monitored and control...

Страница 43: ...nt set up and running samples You will find step by step instructions for common operations in the ICP Expert Help To access this information 1 Double click the ICP Expert Help icon on the desktop 2 When the ICP Expert Help appears click How to to view the available step by step instructions Analysis Checklist You need to complete the following steps in turn to measure a sample s You will find inf...

Страница 44: ...CP OES instrument and that the air filter is not blocked 2 Turn on the laboratory exhaust system 3 Ensure the gas and water lines are connected to the ICP OES instrument 4 Switch on the water cooler 5 Turn on the gas supply 6 Ensure that the gas and water supplies are turned on and set to the correct pressures and that the water cooler is set to the correct temperature 7 Check that the torch is cl...

Страница 45: ...Expert software The Main Index window will appear Running the instrument from an idle state During an idle state both power switches are On the polychromator temperature is regulated and polychromator gas purge is running to ensure the instrument is ready for analysis within 20 minutes after lighting the plasma To begin using the instrument from an idle state 1 Turn on the laboratory exhaust syste...

Страница 46: ...rging the polychromator can take up to several hours The polychromator thermal stabilization can take up to several hours from long term shutdown 2 Ensure that the peristaltic pump is correctly set up refer to the Peristaltic Pump section of the ICP OES Familiarization DVD or the ICP Expert Help If you have not already done so adjust the pressure bars on the peristaltic pump for even sample flow a...

Страница 47: ... will be displayed Otherwise you may Browse for more files The Open dialog box will be displayed in this instance Creating a new worksheet from a template To create a new worksheet from a template click New From on the Start page or New From Template from the File menu A list of recently used files will be presented otherwise you may Browse for more files The New From Template dialog box will be d...

Страница 48: ...ytical lines close to the selected analytical line Their relative intensity will govern how close the lines can be to each other For example if your matrix contains an element that is not of analytical interest but is a potential interferent and has a line close to one of your analytical lines the concentration of that element in your matrix will determine whether you need to choose another analyt...

Страница 49: ...you are using an autosampler click the Autosampler tab to select the racks and probe depth if needed Depending on the autosampler selected options may vary NOTE See the ICP Expert Help or ICP Expert eFamiliarization DVD for a more detailed description of setting up a method Running Samples To run samples 1 Set up the autosampler with all solutions if required 2 Click the Analysis tab and do the fo...

Страница 50: ...ge of pages Reports are printed to your default printer unless you specify otherwise You can specify your printer options in the Print Setup dialog box accessible from the File menu Instrument Idle State In between routine use it is recommended the instrument be left in the idle state which is when the instrument is fully powered but the plasma off In this state the polychromator thermostating sys...

Страница 51: ...r Boost on the Status tab on Instrument window This is not recommended if you are routinely analyzing lines below 190 nm as the instrument will take some time to stabilize when the polychromator boost is turned on again 4 To increase the pump tubing lifetime loosen the peristaltic pump tubes by releasing the pressure bars and lift the tubes out of the grooves To do this a Push up the pressure bar ...

Страница 52: ...ted gas purge to the polychromator assembly during the run and idle states only to minimize the ingress of moisture It is recommended that both the instrument and gas supplies be left on at all times except during long periods of non use 1 Follow Steps 1 6 of the idle state procedure 2 Switch off any accessories where applicable and then shut down the argon gas supply at the cylinder 3 Switch off ...

Страница 53: ...take several hours due to the gas purge and polychromator thermal stabilization time NOTE If the instrument is not going to be in use for a period of time the torch cone snout and torch compartment should be cleaned of any deposits dirt or residue Check the cleanliness of the removable axial window when cone is removed ...

Страница 54: ...Operation 54 Agilent 5100 and 5110 ICP OES User s Guide This page is intentionally left blank ...

Страница 55: ...r should be carried out only by Agilent trained Agilent qualified or Agilent authorized field service engineers WARNING Eye Hazard Always wear appropriate safety glasses when handling sample solutions and other chemicals or when the plasma is on in order to minimize the risk of eye damage by hazardous liquids and exposure to ultraviolet rays WARNING Shock Hazard This instrument contains electrical...

Страница 56: ...nuals for their maintenance procedures and to the ICP Expert Help for the maintenance procedures for any accessories you ordered Routine The following parts of the ICP OES consumables and accessories require routine maintenance Maintenance instructions are included in the ICP OES Familiarization DVD and the ICP Expert Help To access these instructions click the Maintenance tab on the DVD or double...

Страница 57: ...ter cooler for details Check clean the heat exchanger radiator on the cooling system to remove any build up of dust and dirt Perform an instrument calibration Inspect the external gas supply system for leaks including the tubing connected to the instrument and stress cracks Replace any damaged leaking or worn components Annually Clean the water filter Drain and replace chiller coolant Replace the ...

Страница 58: ...r representative to confirm that the proposed method will not damage the equipment Torch Cleaning See the ICP Expert Help for instructions on how to clean the torch for organic based samples and have carbon build up on the injector To access the Help double click the ICP Expert Help icon on the computer desktop WARNING Hot Surface and Chemical Hazard The torch and torch compartment become hot duri...

Страница 59: ...me required for the cleaning procedure will depend upon the extent of the contamination Do not leave the torch in the acid for longer than 8 hours IMPORTANT For one piece torches use a clean wide diameter open top beaker or a similar container to hold the torch inverted while soaking in acid For two piece demountable torches Use a large enough beaker or similar container to fully submerge the torc...

Страница 60: ... the plastic base Damage to the seals and torch body may occur NOTE A torch cleaning stand is available from Agilent which helps keep torches upright and steady during cleaning See the Agilent website www agilent com for details 3 Keep the one piece torch inverted through all the cleaning and rinsing steps unless otherwise directed Figure 13 A One piece torch in acid and B demountable torch body w...

Страница 61: ...utside of the torch with deionized water 18 MΩ cm using a wash bottle to direct the water stream See Figure 15A and B 3 Invert the torch see Figure 15C so that the quartz tubes are at the top and the ball joint connector is at the bottom Direct rinse water through the quartz tubes so that the water flows out of the gas entry ports and ball joint connector for at least 30 s Figure 15 A Rinsing the ...

Страница 62: ...he ball joint connector at the top See Figure 16A 2 Blow clean compressed air or nitrogen through the three gas supply ports two on the base and through the ball joint connector to remove moisture 3 Ensure that all moisture is removed before refitting the torch into the instrument Figure 16 A Drying the torch upper gas supply port B Close up shows drying through the lower gas supply port C Close u...

Страница 63: ...ng may lead to discoloration of the plastic base This change is cosmetic only and should not impact performance if the torch is clean and the results of the other torch checks are satisfactory Store the torch in the original box or a plastic bag when not in use Troubleshooting For troubleshooting information please see the ICP Expert Help 1 Double click the ICP Expert Help on the computer desktop ...

Страница 64: ...r inlet filter basic Air inlet filter dust filter Axial pre optic window Radial pre optic window Spray chamber Nebulizer Peristaltic pump tubing Drain tubing Technical Support For technical support contact information refer to the Agilent Technologies website for details www agilent com ...

Страница 65: ......

Страница 66: ...anual describes the following Safety Practices and Hazards Introduction Installation Operation Maintenance and Troubleshooting Agilent Technologies 2014 2016 2017 2018 Printed in Malaysia 7 18 G8010 90002 G8010 90002 G8010 90002 Issue 6 ...

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