Agilent Technologies 5800 ICP-OES User Manual Download | Manualshive

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Operation

Agilent 5800 and 5900 ICP-OES User's Guide

39

4

Operation

Analysis Checklist

39

Turning On the Instrument and Software

40

Preparing for Analysis

41

Performing a Detector and Wavelength Calibration

42

Creating/Opening a Worksheet

42

Developing a Method

43

Running Samples

45

Printing a Report

45

Turning Off the Instrument

46

This chapter provides a quick guide to getting the instrument 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 and Learning Center 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 information on each step in this chapter.



Turn on the PC, instrument and software



Connect the software to the instrument



Prepare for analysis



Perform a dark current scan and wavelength calibration



Create/open a worksheet

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Summary of Contents for 5800 ICP-OES

Page 1: ...Agilent 5800 and 5900 ICP OES User s Guide ...

Page 2: ...covering the material in this document that conflict with these terms the warranty terms in the separate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license Restricted Rights Legend U S Government Restricted Rights Software and technical data rig...

Page 3: ...Symbols 12 2 Introduction 15 Site Preparation Requirements 15 User Documentation 15 Conventions 16 Notes and tips 16 ICP OES Argon Gas Supply 16 Exhaust System 17 ICP OES Instrument Cooling Air Supply 17 Water Chiller System 18 Drain Vessel 18 3 Installation 19 Agilent ICP OES Instrument Overview 20 Instrument Status LED Color Coding 22 Front Power On Off Button 22 ICP Expert Software 23 Connectin...

Page 4: ...e System AVS AVS 4 AVS 6 and AVS 7 36 External Inlet Duct Adapter 36 Vapor Generation Accessory VGA 36 Multimode Sample Introduction System MSIS 36 Argon Humidifier 37 IsoMist Programmable Temperature Spray Chamber 37 4 Operation 39 Analysis Checklist 39 Turning On the Instrument and Software 40 Turning on the instrument for the first time or from long term shutdown 40 Running the instrument from ...

Page 5: ...n off 46 Setting the instrument to Standby Mode with argon on or off 47 Turning off the instrument for long term shutdown 48 5 Maintenance and Troubleshooting 51 Routine 52 Cleaning 54 Torch Cleaning 54 Important 55 Acid soak cleaning procedure for the torch for aqueous or acid based samples one piece and semi demountable torches 56 Rinsing the torch 59 Drying the torch 61 Additional checks after ...

Page 6: ...Contents 6 Agilent 5800 and 5900 ICP OES User s Guide This page is intentionally left blank ...

Page 7: ...se 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 potential hazards If the instrument is used in any manner not specified by Agilent this protection provided by the equipment may be impaired It is good p...

Page 8: ...ma The plasma is extremely hot about 10 000 C and radiates dangerous levels of radio frequency RF and ultraviolet UV energy The work coil operates at 1 500 V RMS and about 27 MHz Exposure to the RF and UV energy can cause severe skin damage and cataracts of the eyes while close contact with the operating plasma can result in severe heat burns to the skin and an electrical discharge that can jump a...

Page 9: ...ment Use only torches and related components supplied or authorized by Agilent Heat Vapors and Fumes Heat ozone vapors and fumes generated by the plasma can be hazardous and must be extracted from the instrument by means of an exhaust system Ensure that an exhaust system of the appropriate type is fitted as specified in the Site Preparation Guide The system must be vented to the outside air in acc...

Page 10: ...ories Use only instrument grade gases with your spectrometer If using cryogenic gases for example liquid argon prevent severe burns by wearing suitable protective clothing and gloves Electrical Hazards The spectrometer system and some accessories contain electrical circuits devices and components operating at dangerous voltages Contact with these circuits devices and components can cause death ser...

Page 11: ... the hazards associated with use of the acids used for sample preparation and apply all necessary precautions including use of lab coats safety goggles and other appropriate forms of personal protection The acid wastes should be disposed of in accordance with local regulatory requirements The type volatility and concentration of the organic solvents used in the sample that is measured varies depen...

Page 12: ... The following is a list of symbols that may appear in conjunction with warnings in this manual or on the spectrometer The hazard they describe is also shown The beginning of the warning text is noted by a warning icon WARNING A triangular symbol indicates a warning The meanings of the symbols that may appear alongside warnings in the documentation or on the instrument itself are as follows Broken...

Page 13: ...rect procedure referred to by that warning label The following symbols appear on the instrument for your information I Mains power on 0 Mains power off Single phase alternating current Protective ground terminal Socket for Agilent accessory serial cable Socket for Ethernet LAN cable Socket for Agilent accessory USB cable Indication of correct orientation of gas filter flow direction Caution discon...

Page 14: ...Safety Practices and Hazards 14 Agilent 5800 and 5900 ICP OES User s Guide This page is intentionally left blank ...

Page 15: ...aboratory 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 If you have misplaced your copy you can obtain a free replacement from your local Agilent office Position the equipment for easy access to the disconnecting switch on the left side of the instrument User Docume...

Page 16: ...the F2 key and text you must type in from the keyboard e g type SETUP at the prompt Notes and tips A Note is used to give advice or information A Tip is used to give practical hints to help you achieve the best possible performance from your ICP OES ICP OES Argon Gas Supply Table 1 Typical flow rates for the Agilent ICP OES instruments Typical Flows Argon with nitrogen purge gas Measuring waveleng...

Page 17: ...a dust filter to filter out particulate matter The air supply is used to cool the internal mechanical and electronic components of the instrument Several of these assemblies contain parts prone to corrosion The introduction of cooling air contaminated with high levels of acid vapors or other corrosive substances may cause damage to the instrument Due to the corrosive nature of some analytical work...

Page 18: ...rument drops below 1 7 L min 0 45 gpm A second water flow sensor will stop the camera Peltier cooling assembly if the water flow through the instrument drops below 0 2 L min 0 05 gpm CAUTION Always ensure the water chillersystem is on before igniting the plasma Drain Vessel The Agilent ICP OES system needs a drain vessel for disposal of excess fluids from the spray chamber or autosampler Suitable ...

Page 19: ... Disassembly 27 Accessories 35 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...

Page 20: ...xial viewing window not shown 10 Nebulizer 17 Optics purge filter for argon or nitrogen 4 Snout and radial viewing window not shown 11 Peristaltic pump 18 Gas supply assembly 5 Work 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 connectio...

Page 21: ...er 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 shielded 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 nitrogen ga...

Page 22: ...ndle 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 normal instrument operation User intervention is required to resolve...

Page 23: ...rk Flat File Standalone or network Database for 21 CFR Part 11 installations Upgrading Standalone or Network Database ICP Expert installations Installation includes Installing the ICP Expert software Installing the ICP Expert Help Installing the LAN cable Setting the instrument IP address Installing and configuring SDA for 21 CFR Part 11 compliance Installing and configuring SCM for 21 CFR Part 11...

Page 24: ...oftware and open the Instrument Window 3 Connect the software to the instrument if needed a Click Instrument in the ICP Expert toolbar b Click Connect c Select the instrument from the list and the click Connect 4 Click Calibrate in the Detector section NOTE Once the detector calibration is completed the date and time of the last successful calibration will be displayed confirming the detector meas...

Page 25: ...and time of the last successful calibration will be displayed a pass or fail mark will appear along with the wavelength error indicating whether the instrument calibration is complete Saving and viewing the calibration data The calibration data is stored in the Logs To view the data export the Logs 1 From the main ICP Expert window click File Logs Export Logs 2 Save the zipped Log file 3 Open the ...

Page 26: ...m with slot Medium with slot Medium with slot Medium with slot Outer tube material Quartz Quartz Quartz Quartz Intermediate tube 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 Parameter Radial View Torches Standard torch Semi demountable torch Inert semi demountabl...

Page 27: ...ts e g ketones kerosene Jet A1 Volatile organic solvents e g gasoline A fully demountable torch can be adapted for another application by replacing the injector and or the outer tube with the configuration recommended for that sample type Refer to the Agilent Technologies website for ordering information Torch Assembly and Disassembly Both the semi and fully demountable torch models allow the oute...

Page 28: ...ious amounts of water and seek medical attention immediately CAUTION To prevent damage to the torch always take care when handling or storing it To prevent damage to the instrument do not use the torch if it is damaged or wet Figure 3 Demountable torch where 1 Torch 2 Top seal and 3 Torch body Assembly of the semi demountable torch To assemble the torch 1 Place the top seal back on the quartz tube...

Page 29: ...d to the quartz outer tube set 2 Slide the top seal approximately 1 3 the way up the quartz tube set and position it so the top face of the seal is aligned with the bottom of the T alignment mark as shown in Figure 5 Figure 5 The top seal aligned with the alignment mark on the quartz outer tube ...

Page 30: ...Position the quartz tube set so that the groove on the torch body aligns with the T alignment mark on the quartz tube set as shown in Figure 7 Figure 7 The alignment mark on the quartz outer tube set should be aligned with the groove on the torch body 5 Press the quartz outer tube set fully into the torch body and then press down on the top seal to secure the tube set in place See Figure 8 ...

Page 31: ...ated by pressing firmly on the top edges 3 Insert the tube set into the torch body and position it so that the groove on the torch body aligns with the T alignment mark on the tube set Press the outer tube set fully into the torch body See Figure 7 and Figure 8 4 Fully insert the injector through the base of the torch body until the bulge contacts the retaining arm and clicks into position 5 Repla...

Page 32: ...ring from the torch body if you are unable to do so by hand 1 Gently loosen the top seal either by prodding it using thumb nail see Figure 9 or use a wide blade flat screw driver to lever it up When using a screw driver insert the screw driver into the slot as shown in Figure 10 maintaining an up down action to lever the seal loose Repeat the action on the opposite slot The seal should be dislodge...

Page 33: ...op seal with an aid of a wide blade flat screw driver 2 Maintaining a straight parallel movement carefully slide the quartz outer tube set off the torch body See Figure 11 Figure 11 Removing the quartz tube set from the torch body Avoid contact between the quartz tube set and injector ...

Page 34: ...re 12 Removing the top seal off the quartz tube set To disassemble the fully demountable torch 1 Unscrew the locking nut on the base of the torch and remove the injector by gently pulling on the ball joint 2 Remove the quartz tube set from the top of the torch base If the top seal is removed with the quartz outer tube set slide the top seal off the tube set towards the top end ...

Page 35: ...m MSIS Argon humidifier IsoMist Programmable Temperature Spray Chamber For safety and installation information please see the accessory documentation or the ICP Expert Help and Learning Center SPS 4 See the instructions that came with the accessory for safety information and to prepare the SPS 4 for installation The SPS 4 is compatible with a wide range of commercially available low cost autoclava...

Page 36: ...mple analysis times are reduced The AVS 6 and AVS 7 include a bubble injector that automatically injects bubbles after the sample is loaded into the loop isolating the sample from the rinse carrier solution This reduces the volume of sample required for measurement therefore reducing analysis time as tailing or dilution effects are minimized External Inlet Duct Adapter The External Inlet Duct Adap...

Page 37: ...with high dissolved solids or high dissolved salt content When using the accessory the nebulizer gas flow is passed through the humidifier to increase the water vapor in the gas This has been found to be beneficial by reducing the build up of salt and other dissolved solids in the nebulizer tip in the sample introduction system By reducing blockages the Argon Humidifier helps to ensure uninterrupt...

Page 38: ...Installation 38 Agilent 5800 and 5900 ICP OES User s Guide This page is intentionally left ...

Page 39: ...g 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 and Learning Center 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...

Page 40: ... Turn on the laboratory exhaust system 3 Ensure the gas and water lines are connected to the ICP OES instrument 4 Turn on the gas supply 5 Switch on the water chiller 6 Ensure that the gas and water supplies are turned on and set to the correct pressures and that the water chilleris set to the correct temperature 7 Check that the torch is clean and in good condition and installed with the torch ha...

Page 41: ...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 standby state 1 Turn on the laboratory exhaust system 2 Check that the torch is clean and in good condition and installed with the torch handle fully closed 3 Check that all tubing on the spray chamber nebulize...

Page 42: ...at the peristaltic pump is correctly set up refer to the Peristaltic Pump section of the ICP Expert Help and Learning Center If you have not already done so adjust the pressure bars on the peristaltic pump for even sample flow and drainage 3 Place the sample tubing from the peristaltic pump into the rinse solution and the drain tubing into the drainage vessel 4 Click the Pump button in the ICP Exp...

Page 43: ...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 displayed in this instance The Worksheet window will appear with the new worksheet loaded Developing a Method NOTE For instructions on how to configure and use accessories IntelliQuant and Extended QC options see the ICP Expert Help and Learni...

Page 44: ...lytical line 5 Make any required adjustments to each element including selecting a different wavelength entering additional information into the Label column and selecting the type choose from analyte internal standard or interferent 6 Click Conditions to modify both common settings for the run and settings for each element Up to eight different measurement conditions can be used 7 Click QC to ent...

Page 45: ...select all solutions select the checkbox next to the Rack Tube title b Click the Run icon in the toolbar or press the SHIFT F8 keys to begin the analysis and follow the prompts NOTE For further information about running an analysis refer to the ICP Expert Help and Learning Center Printing a Report To print a report 1 Click Report on the toolbar or File Report 2 Choose whether you want to print or ...

Page 46: ...0 ICP OES in a state of readiness while only consuming low amount of utilities argon gas and electricity The benefit of being in Standby Mode is the 5800 5900 can be operational again in 20 minutes from plasma ignition Standby Mode is automatically enabled once the previous analysis is finished and the plasma is shut down Follow Setting the instrument to Standby Mode with argon on or off on Page 4...

Page 47: ...gon gas is turned back on NOTE If you are turning off the argon gas also turn off the water chiller Setting the instrument to Standby Mode with argon on or off To put the instrument into Standby Mode 1 Rinse the spray chamber by aspirating water for a few minutes NOTE When running organic samples it is recommended that the spray chamber be cleaned and dried thoroughly between analyses 2 Extinguish...

Page 48: ... the printer monitor and any accessories if desired Ensure that the Powersave option on your PC is disabled this will prevent the shutdown of your hard disk If this option is not disabled you could lose data during an unexpected shutdown WARNING Noxious Fumes Inhalation danger The exhaust system MUST remain on if the gas supplies are on Turning off the instrument for long term shutdown For extende...

Page 49: ... front power on off switch green LED to stop blinking and then switch off the mains power switch on the left side of the instrument This will turn off the complete instrument as well as the polychromator thermostatting system 5 Turn off the laboratory exhaust system 6 Exit the ICP Expert software if it is no longer required by choosing Exit from the File menu Switch off the printer and monitor Res...

Page 50: ...Operation 50 Agilent 5800 and 5900 ICP OES User s Guide This page is intenionally blank ...

Page 51: ...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...

Page 52: ...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 Expert Help and Learning Center To access these instructions double click the ICP Expert Help and Learning Center icon on the computer desktop Click on or search for Maintenance The frequen...

Page 53: ...he spray chamber Clean the nebulizer Check the other sample introduction and transfer tubing and O rings look for excessive wear poor sealing or kinks and replace as necessary Inspect the removable axial and radial pre optics windows for cleanliness Clean or replace as necessary Check the condition of the filter in the air inlet on top of your instrument Remove the air inlet filter assembly and re...

Page 54: ...ary this cloth can be dampened with water or a mild detergent Do not use organic solvents or abrasive cleaning agents Before using any cleaning agent procedure or decontamination method except those specified by Agilent the user or other authorized personnel should check with your local authorized Agilent field service engineer or representative to confirm that the proposed method will not damage ...

Page 55: ...emovable top seal of semi demountable torch Keep the torch vertical with the ball joint at the top throughout all cleaning and rinsing steps unless otherwise directed Do not remove the torch adhesive cap on the one piece torch that covers the seal between the quartz and the plastic For a better clean always disassemble the semi or fully demountable torch during rinsing and drying procedures WARNIN...

Page 56: ...ime required for the cleaning procedure will depend upon the extent of the contamination Do not leave the torch in the acid for longer than 4 hours If deposits remain after using 50 Aqua Regia repeat the cleaning process using a higher concentration of Aqua Regia 4 Place the torch in the aqua regia solution through the hole provided in the torch cleaning stand as shown in Figure 15A B C and D Ensu...

Page 57: ...h 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 6 Keep the one piece torch inverted through all the cleaning and rinsing steps unless otherwise directed Figure 15A Soak the torch in the aqua regia solution Ensure the injector is immersed in the solution ...

Page 58: ... stand with swappable torch plates Injector soaking in aqua regia Figure 15D Quartz outer tube set soaking in aqua regia 7 Rinse the torch and outer tube set thoroughly and dry completely prior to using the torch in the instrument 8 Follow the steps outlined below for Rinsing the torch and Drying the torch listed below ...

Page 59: ... the torch with deionized water 18 MΩ cm using a wash bottle to direct the water stream See Figure 16A 3 Invert the torch see Figure 16B so that the quartz tube or injector are at the top and the ball joint connector is at the bottom Flush rinse water through the quartz tubes so that the water flows out of the gas entry ports and ball joint connector for at least 1 minute Figure 16A Rinse the inje...

Page 60: ...r 4 If the torch was disassembled for cleaning thoroughly wash the quartz outer tube set and the removable top seal See Figure 17A and Figure 17B Figure 17A and B Rinse the quartz outer tube set and top seal with deionized water 5 Dry the torch completely and re assemble the semi demountable torch if necessary prior to using the torch on the instrument ...

Page 61: ...rying the torch below This extra step can help to reduce deposition on the outer tube of the torch CAUTION Do not place the plastic parts of the torch in a drying oven It is not as effective at removing moisture as using compressed air argon or nitrogen and may damage the torch Drying the torch 1 Hold the torch inverted with the ball joint connector at the top 2 Blow clean compressed air argon or ...

Page 62: ...gh the quartz outer tube set and top seal to remove all moisture 5 Carefully blow away any moisture left on the body of the torch and quartz parts 6 Ensure that all moisture is removed before refitting the torch into the instrument 7 For the semi and fully demountable torch it is advisable to disassemble the torch giving easy access to the torch body for complete drying Additional checks after cle...

Page 63: ... is clean and the results of the other torch checks are satisfactory TIP Store the torch in the original box or a plastic bag when not in use or alternately use the Agilent ICP OES Easy fit torch storage rack P N G8010 67000 Troubleshooting For troubleshooting information please see the ICP Expert Help and Learning Center 1 Double click the ICP Expert Help and Learning Center on the computer deskt...

Page 64: ...t of recommended spares to keep on hand to minimize downtime during maintenance and repairs Torch one piece or spare components such as the outer tube set and injector if using a demountable torch Air inlet filter element dust filter Axial pre optic window Radial pre optic window Spray chamber Nebulizer Peristaltic pump tubing Drain tubing Technical Support For technical support contact informatio...

Page 65: ......

Page 66: ...wing The manual describes the following Safety Practices and Hazards Introduction Installation Operation Maintenance and Troubleshooting www agilent com Agilent Technologies Inc Agilent Technologies 2019 Edition 1 10 2019 G8020 90002 G8020 90002 ...

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