Home

AAnalyst 200 User's Guide

1. eeeeeesesseeeseeensecnsecesecesecsseeeseeeseeeeeeesnes 7 25 Tools Diala ninne neen E e E vb ee evs 7 27 Recommended Conditions ee eeeeeseeeseeeseeeseecesecesecesecsseesseeeeeeeeeeeeaes 7 31 Network Dialog sidruni Gees be eetedeas oda dev toa E a 7 32 Download orie ween oie aie eee es 7 41 Importing AAnalyst 200 into Microsoft Excel 7 47 Chapter 8 Analyzing Samples Sequence Of Operations ys 0 1 sci eesietetietstwestie steeds eis steieteeteatvaeeniessindoeeece 8 3 Manual Flame Analyses 0 0 ce eeceescecsecsseceseceseceseeeseceseeeseeseeeesaeeeaeesaaeenaees 8 4 Automated Flame Analyses cece ceecescceseeeseeesseceseceseceaeceseeeseeeseeeeeeeenes 8 15 Manual Analyses Data Display MHS Technique eee eeeeeeeeeereeeeee 8 22 Running Samples in Emission Mode e cc eeeesseesseceseceseceeeceeeeeseeeeeeeenes 8 23 Shutting Down The System cece ceseceseceseceseceeeceeeeeseeseneeeseeeaeeesaeenaees 8 31 Emergency SHUtd Owais ssss20 cstsse casei veresectesnrsedevs cst eiee erer er en T 8 32 Rinsing the Burner System ee ee eeseeesceeseeencecaeceseceaecsseeeeeeeseeeseeeeaes 8 33 Chapter 9 Maintenance IntrodctiOn cenae aa oe eed ede e cee 9 3 General Maintenance Checklist ee eeeeeeeeseeeneeeeeeeecaecsseceaeesseenseeees 9 4 Instrument Maintenance Checklist ee ceeceeecseeeeeeeeseecseecsseceaeceaeenseeess 9 5 CHECKS visi isiedoslszscebselasceesushaute laSercaehsseccesselavoat EE EE 9 7 Spectrometer Maintenance Che
2. To establish connection between a stand alone computer and the AA200 instrument follow the procedure below It is recommended that you contact your system administrator to setup connections for network computer Stand Alone Computer 1 Use a crossover cable P N 0941 0061 to connect the AA200 instrument to a computer e Connect the crossover cable to the Ethernet port of the E Box see chapter 5 for connectors on the E Box e From the E Box run the crossover cable to the Ethernet port of the computer 2 From the AA application Touch Screen touch the Tools button to access the Tools dialog 3 Touch the Network button on the Tools dialog to access the Network dialog Oktoin an IP address via DHCP Instrument ID Specity an IP address Password Screen 7 19 Network Dialog 4 At the top of the Network dialog click on the Store Data on Network Drive check box to turn the store data function on 7 32 AAnalyst 200 User s Guide Network Setup 5 Inthe Network Setup section of the Network dialog choose Specify an IP address option Enter the suggested IP Address and Subnet Mask below e IP Address 10 0 0 1 e Subnet Mask 255 255 255 0 NOTE Entries for Default Gateway are not needed for a stand alone computer Storage Location In the Storage Location section of the Network dialog fill in the entries for Computer Name Share Name User Name and Password 6 Computer Name Enter the
3. cece ceeceseeeeeeeeee 4 21 Chapter 5 Installation Introduction to the Installation Procedure ee ee esceessecneesseceseceeesseeees 5 3 When the Spectrometer Arrives eccesceseceseceseceseeeeeeeseeeeeeeeaeeeseeeaaeeaeens 5 4 Placing the Spectrometer on the Bench ee eeeeeeeeeseeeseceseceseceseenneeees 5 6 AAnalyst 200 Shipping List 2 0 eeceeseeeeneeeeeeeeeseecaecaecsaeeeseesaeenes 5 8 AAnalyst 200 Spares Kit ccccucccetecessceesscesseseneceecsesteconteersoderseestectneceesa 5 9 Installing the Touch Screen oo cece ceeceeeceseeeeeeeseeeseeeaeceaeesseeeeeeeseeeseeeeaes 5 10 Connecting the Gas Hoses cc c cs cessaseuesctccesensteievescdocteesstsdevssetesedearteledestts 5 14 Setting up the Burner System oo eee iseina ii 5 19 Installing the Burner Doot ee ee eeeeeeeeeseeeseeeseecaeceseceseceseeeseeeseeseeeeenes 5 21 Installing the Sample Tray ee ceeceeseesceeseeeseecesecesecesecsseceseeeeeeeneeeeaes 5 22 Connecting to the Electrical Supply 2 0 0 0 cee ecccceesseceeeeeeeteeeeeeeeeeceeeeeesas 5 23 Switches and Connectors on the E BoX 0 ee eeceeceeseeeeeeeeeeeeeeeeeneeenaees 5 24 Setting Up the AutoSamplet eee ceeesecsseceseceeeceseeeseeeeeeeeaeeeaeeeaeenaees 5 25 Connecting the Foot Switch oo eee eeeeseeeseeencecsaeceseceaecsseeeseeeseeeneeeeaes 5 26 Chapter 6 Operation of Instrument Starting up the Systems sich eiaiieani antl EEE VEE A Ei 6 3 Setting up the Burner System e
4. damage the burner chamber or drain tubing To flush the system remove the burner head then slowly pour about 500 mL of water into the burner chamber Allow the water to drain into the drain vessel Replacing the Drain Tubing If the drain tubing P N 0250 7987 is damaged or extremely dirty and needs to be replaced refer to the next figure and proceed as described next Burner End Cap Burner Assembly Drain AN Fitting al t Drain Clamp ane Drain ubing f Interlock ie S _ Plug y Drain Interlock Connector Drain Interlock Cable Figure 9 11 Replacing the drain tubing Dispose of drain vessel waste in accordance with the regulations applicable to your locality state and or country WARNING 9 33 NOTE Maintenance P amo ia Turn off the AAnalyst 200 power switch Empty the drain vessel Unplug the drain interlock connector from the burner see Figure 9 11 Remove the spiral wrap from the drain tubing by unwrapping it This will release the drain interlock cable Disconnect the drain tubing from both the drain vessel and the drain outlet on the burner end cap by loosening the clamps on each end of the tubing Once the clamps are loosened the tubing should easily pull out Place the new piece of drain tubing P N 0250 7987 next to the drain interlock cable and carefully rewrap the spiral wrap around them both Place the drain clamp on the upper end of the new drain tubing Then attach the tubing to
5. ec ceeeeeceeeeeeees 9 5 9 6 manual analyses continuous display ee eeeeeeeeeee 8 11 data display eee eeeeeeceseeeeeee 8 4 8 6 data display MHS technique 8 22 mercury hydride determination system ALOMIZELS A ox h Mechs ceeds arenes 4 21 MHS 10 see Mercury Hydride Determination System eee 4 21 N nebulizer ACJUSTING eee eee ii 9 35 leai eneit 9 32 9 37 cleaning sample tube 9 32 clearing an obstruction 9 32 COMPONENTS eee eeeeeseceseceseceteeeeeeeees 9 52 disassembly 9 33 installing somission 6 6 9 27 installing in end cap s es 9 28 impact bead removing and replacing 9 34 maintenance checklist eee 9 9 OATIN AA AE eee Acne 9 39 OpPtMIZIN S notae raie reote 6 40 preadjustih Sis siropini oiite 6 37 reassembling seere 9 38 nitrous oxide CONNECUNG onien ne 5 17 cylinder information eee 3 18 heated regulator s 3 18 requirements eeeeeeererereereerereeee 3 17 WalNINGS noroi z bse ae e ee lee 3 17 O o rings burner system o0 cele eee eeeeeeeeereees 9 39 maintenance checklist eee 9 9 operating conditions environment niesie ieat 2 18 operational on off switch location 6 25 optimization procedures eee 6 28 burner system o ee eee eeeeeeereeeneees 6 39 gas TOWS 2 0 irienna 6 41 NE DUI ZeL svete siesieecdeieeshietidee eth 6 40 organic solvents 9 36 oxidant flow entry on flame page eee 7 12 P periodic checks 0
6. Setup Instrument Wavelength nm 0 00 Slit ram Install Lamps ane Screen 8 15 Lamp page In the Signals dialog touch the Flame Emission radio button to change the signal to Flame Emission Touch the OK button to close this dialog box Once the dialog box closes the element field will become blank Select an appropriate element for analysis A dialog box will then appear telling you to aspirate the most concentrated standard Place the tubing in this standard and press the OK button The gain setting for the element will be based on this highest standard 8 25 Analyzing Samples Signal Set Midscale Atomic Absorption Element Background Corrected AA Cancel Setup Instrument Wavelength nm Flame Emission Slit mm Install Lamps Parameters Analyze Tools Screen 8 16 Lamp page Signal Dialog 7 Complete the Flame page Enter the required flame type the oxidant and acetylene flow for the element to be analyzed 8 26 AAnalyst 200 User s Guide Bleed Gases Oxidant air Auto Scale Graph Auto Zero Graph Oxidant Flow L min A joo gt _ suo zero craon_ On Off Z Acetylene Flow L min a 2 50 La Interlocks Parameters Analyze Tools Screen 8 17 Flame page 8 Select the Parameters page Spectrometer tab Use the appropriate values to fill in the settings 8 27 Analyzing Samples I on 1 a EN h N R n Screen 8 18 Parameters page Spectrometer t
7. 7 Close the compartment door 9 48 AAnalyst 200 User s Guide Figure 9 16 Replacing the E Box 9 49 Maintenance Maintaining the Acetylene Supply Warning Acetylene Explosion Hazard Acetylene can decompose explosively at pressures higher than 103 kPa 1 03 bar 15 psig Always make sure that the acetylene outlet gauge pressure is below this value Depressurize both the fuel and oxidant gas hoses at the end of the working day or if you are not going to use the instrument for an extended period Close the cylinder valves to avoid the possibility of gas hoses being subjected to the full cylinder pressure in the event that a pressure regulator should fail Acetylene is supplied dissolved in a solvent such as acetone and a small amount of solvent carryover with the acetylene is normal However as tank pressure falls the relative amount of solvent entering the gas stream increases and can give erratic results particularly for elements such as calcium tin chromium molybdenum and others whose sensitivity is highly dependent on the fuel oxidant ratio The pressure drop is not linear with gas removal since the acetylene is dissolved in a solvent and a pressure of 600 kPa 6 bar 85 psig at ambient temperature indicates that the cylinder is nearly empty For this reason replace acetylene cylinders when the cylinder pressure drops to about 600 kPa 6 bar 85 psig Always store and use acetylene
8. A AAnalyst 200 feature Sanne Ree ent a neii 4 5 OVELVICW eae er E e 4 4 acetylene CONMECUNG iioii i ie i 5 18 cylinder information eee 3 18 flash arrestor sosise 3 19 STAI eis siete e a hh atest 3 18 requirements and safety ee 3 18 Sate USE cscchers tet a re aie 3 19 tubing and fittings eee 3 19 Warning COPPEL eeeeeeeseeereeeneeeeees 3 18 WaIMINGS soi celeste distin ene 3 18 acetylene flow entry on flame page secese 7 12 acetylene cylinder maintenance checklist 00 0 eee 9 9 addition calibration technique 7 19 analyte addition calibration 0 0 7 19 analyte addition technique 7 18 analyte see element cece eeeeseeneees 7 7 analyze all analyze samples page cece 7 26 analyze blank button on analyze samples page E A E 7 22 7 24 analyze page autosampler oc eeeessecsseceneceeees 7 25 manual data display 7 20 7 24 analyze sample button on analyze samples page 7 24 button on analyze samples page 7 22 analyze sample page manual continous display 7 23 analyze samples analyze samples page 7 26 analyze standard button on analyze samples page wa tected Ul A E scets 7 22 7 24 atomic absorption eseese 7 7 auto scale graph oc eeeeesseceeneeeeeeees 7 24 button on flame page oseese 7 13 auto zero graph button on Flame page eee 7 13 aut
9. Analyze Sample fi Printer On Off Parameters Screen 8 21 Analyze page 8 30 NOTE NOTE NOTE AAnalyst 200 User s Guide Shutting Down The System In an emergency switch off the spectrometer using the operational on off switch behind the front door or use the emergency flame off switch see page 8 32 The flame is automatically extinguished and the gases shut down in a safe sequence Shutting off the Flame 1 With the flame still burning aspirate the correct rinsing solutions to rinse the burner system Either aspirate the solutions manually or use the flame autosampler 2 Touch the Flame tab to display the Flame page 3 Touch the Flame On Off switch 4 The system uses a predetermined shutdown sequence to extinguish the flame safely If a nitrous oxide flame is shut down the system will switched to an air acetylene flame and wait approximately two seconds before automatically extinguishing the flame 5 Shut down the gases to the spectrometer at the source 6 Touch the Bleed Gases button to depressurize the gas lines Shutting off the Spectrometer 1 Switch off the spectrometer at the operational on off switch on the front panel 2 Switch off any accessories 3 Empty the burner drain vessel Dispose of hazardous or corrosive solutions properly and refer to your local safety regulations for proper disposal procedures 8 31 Analyzing Samples Emergency Shutdown If a situation ari
10. Part Number 0303 0152 to find the recommended settings for wavelength slit width and flame type Use these values to make appropriate settings 1 Switch on the AA200 instrument See Chapter 6 Operation of the Instrument 2 The following page is the first page displayed once you start up the system Select the Flame Technique in the Startup screen Touch the Details bar on the screen to get details on the Power on Diagnostics In the Details dialog all entries should be in green to indicate that all systems are OK If all the entries are green touch OK in the Startup screen 3 Turn on the Flame 4 Ifyou want to recall an emission method then do so at this time When prompted aspirate the highest standard of the element being determined This setup solution must be aspirated while the spectrometer wavelength is peaked and the high voltage gain on the photomultiplier is set If you do not have an emission method to recall then proceed to step 5 8 23 Analyzing Samples Signal Element Wavelength nm Slit mm Technique Flame O mhs Set Midscale Power on Diagnostics Setup Instrument All Systems OK Details Install Lamps Enable WinLab32 Control Parameters Analyze Tools Screen 8 14 Lamp page Startup Dialog 5 To change the signal touch the Signal field on the Lamp page A Signals dialog will appear 8 24 AAnalyst 200 User s Guide Signal atomic Absorption Set Midscale Element
11. Replace the drain clamp and tighten securely Installation of the burner drain is complete Installing the Lamp Compartment Door Locate the lamp compartment cover if it is not already on the instrument Install the cover by following the procedures below 1 Hold the door in place next to the lamp compartment as shown below 2 Gently push the upper part of the door on to the upper pin and maneuver the lower part of the door over the screw hole Tighten the securing screw with a screwdriver 3 Close the door 6 17 Operation of the Instrument Lamp Door instrument With Tilt the top of the door Door Removed 1 toward the upper door bracket next to the lamp compartment Maneuver the lower 2 part of the door over the screw hole Tighten Lamp Door in Place Figure 6 9 Installing the lamp compartment cover 6 18 AAnalyst 200 User s Guide User Interface Signal Atomic Absorption Set Midscale Element Cu Setup Instrument Wavelength nm 324 75 Slit mm 2 7 0 8 Install Lamps Screen 6 1 Typical Touch Screen Display Touch screen You operate the spectrometer using the touch screen The touch screen is the interface between you and the spectrometer enabling you to control the spectrometer in order to perform your analyses easily and conveniently The touch screen contains active areas that you touch to perform the required action You may find it more convenient to use a stylus or the
12. You will know that the burner head is fully seated because the ignitor will swing over the burner 4 Let go of the safety latch Look at it closely to confirm that the safety latch hook is positioned over the ring 6 10 AAnalyst 200 User s Guide Installing Solvent Resistant Components in the Burner Warning Flammable Gases Fire and Explosion Hazard Not all gaskets in the burner unit are suitable for use with organic solvents Exposure to such solvents may cause the respective gaskets to swell This may result in a seepage of gas which is a serious fire hazard i 3 WARNING Before you aspirate organic solutions remove the respective gaskets and install solvent resistant gaskets The standard o ring in the burner end cap is not resistant to organic solvents If you intend to aspirate solutions containing organic solvents you must exchange this o ring for a solvent resistant o ring in the following way 1 Where applicable extinguish the flame allow the burner head to cool shut down the gases at source and bleed the gas supply lines 2 Open the atomizer compartment door 3 Remove the burner head 4 If corrosive or toxic samples were run previously pour a large quantity of deionized water slowly through the neck of the burner chamber to thoroughly flush the inside and the drain system 5 Remove the nebulizer from the burner end 6 Remove the burner system from the spectrometer 7 Take the burner ch
13. e The burner Initially you must adjust the burner position so that the burner head is correctly located just below the radiation beam Since the location of maximum atom concentration in the flame varies slightly from element to element you must optimize the burner position while aspirating a suitable standard solution so that the radiation beam passes through the region of the flame containing the highest concentration of free analyte atoms e The nebulizer Initially you must set the solution aspiration rate Since viscosity density and surface tension can influence the aspiration rate to varying degrees you must then optimize the aspiration rate while aspirating a suitable standard solution that has a composition similar to your samples 6 28 AAnalyst 200 User s Guide Aligning Lamp After you have installed the lamp you require for your planned analyses you must align it in the optical path so that maximum radiant energy passes to the detector In a single lamp configuration you must manually align the lamp position by using the adjustable knobs as shown in the figure below Figure 6 14 Lamp alignment controls Warning UV Radiation Risk of Eye Damage The lamps may emit UV radiation which can damage your eyes Do not gaze into a lighted lamp Always wear UV absorbing safety glasses when looking at the radiation from the lamps 6 29 Operation of the Instrument Align the lamp NOTE
14. 0 cee eeeceeeceseeeeeeeeeeees 9 7 plug adaptors oe eee eeeeeereeereeenees 9 53 preconditioning NEW DUHET sisi aegse eest 9 21 new drain tube seere 9 21 pollution degree s 3 20 power entry module COMNECHION iiie ieioi e i ei 5 24 power switch CONNECUON rirse ira e ess 5 24 PLOCAULIONS aissein 2 5 preparing your laboratory environmental conditions 3 4 printer CONMECHON 2i35 He eiieeeeee sions 5 24 R references laboratory safety practice 2 23 remote trigger oseere 5 24 5 26 replacing Crain tubing ee eeeeeeeeneeeeee 9 30 CLE CUCL voces oy es enone 3 20 lani porra e Er cane totes eee 4 10 TOONS aae dhe intents 5 3 replicates s s 5ec ees ceva cssetee n eonen aE TE 7 21 ANALYZE page rererere etie 7 26 dialog in Spectrometer subpage replicates in Spectrometer subpage 7 16 entry on spectrometer subpage 7 16 requirements QD PE ewes ldo Memento Reeieks 3 16 electa hieer eiae 4 19 E E E E eek Ae at 3 15 laboratory sesser 3 7 3 14 DITOU OXIA Ens sessir eritis 3 17 reslope dialog in Calibration subpage reslope in Calibration subpage 7 18 entry on calibration subpage 7 18 result window analyze page seesesreeerereeresreseee 7 25 sample page nenna seeen es 7 21 rinsing the burner system 6 43 8 30 Running Samples in Emission Mode 8 23 RS Dresiisted ices ite Ane eae 7 21 S safety ACELYIENE hai peeked 3 18 acety lidean serasa en is
15. 1 Prepare a blank solution Use the same solvent as you use to prepare the standard solution 2 Prepare a standard solution of the analyte element The concentration of the standard solution should be in the linear range and ideally should be close to the sensitivity check concentration quoted in the Recommended Conditions i e give an absorbance reading of approximately A 0 2 6 39 Operation of the Instrument Optimizing the burner position 1 Touch the Flame tab to display the Flame page 2 Aspirate the blank solution and when the signal is steady touch the Auto Zero Graph button 3 Aspirate the standard solution 4 Adjust the burner position by turning the vertical and horizontal alignment controls alternately and in small increments while at the same time observing the continuous graphics display Continue to make adjustments until you find the position that gives maximum absorbance reading Optimizing the nebulizer In this procedure you optimize the nebulizer aspiration rate for the solutions you will use in the subsequent analyses Warning Flashback Hazard When you optimize the nebulizer using a nitrous oxide acetylene flame WARNING Make small adjustments slowly Do not rotate the adjusting nut more than 1 8 of a turn in total 1 Aspirate the standard solution 2 Turn the nebulizer adjusting nut slowly in very small increments while at the same time observing the continuous graphics display Adjust the
16. 2 Tighten the connection using the double wrench technique Hold the fitting on the air dryer filter assembly with one wrench and tighten the compression nut on the gas hose with the other wrench 5 18 AAnalyst 200 User s Guide Setting up the Burner System Ae a a an Figure 5 9 Full view of the AAnalyst 200 Instrument 5 19 Installation Install the Burner Assembly 1 Carefully remove the foam packing piece from around the burner system 2 Guide the burner assembly into the tracks of the atomizer compartment 3 Push the burner assembly in so that the rear gas fittings line up with the gas connectors at the back of the atomizer compartment Push the burner assembly fully in until it clicks into place and pull the lever forward to lock the burner assembly in place Connecting the Drain Vessel and the Drain Interlock 1 Locate the drain vessel The drain tube and interlock cable will be attached to the drain vessel retainer cap 2 Place the drain vessel in full view on the floor in front of the instrument Never place the drain vessel inside a cabinet 3 Before connecting the drain tube to the burner assembly pour about 250 mL of water into the free end of the drain tube to fill the drain loop and to activate the drain float 4 Place the hose clamp over the free end of the drain tubing 5 Carefully install the free end of the drain tubing over the drain outlet making sure that the in
17. 2 6 n AE EE EA 2 14 high temperatures 0 0 eee eeeeneee 2 6 TOXIC products nisserne es 2 6 UV radiation menines nnne 2 6 WAITING seietara iaee itis 3 17 HCL guetta teen es Chas 4 6 HCL see hollow cathode lamp 6 22 I igniting the flame ee eee eeeeeee 6 35 l 5 Index ignitor descripto iieii oiii i 4 16 installation burner door sssseseeeeseeeeeereeresreererrrees 5 21 burner head oinencncricaisaiiies 6 11 burner solvent resistant components 6 11 burner SySteMm en neinitiati 5 19 electrical supply 5 23 laipsnio e ro ir teeta le ened Meee 6 21 gas HOSES iii dais aes 5 14 placing on bench 5 6 sample Shelf iseis iieis 5 22 shipping St ss ceeccescsscsedeteesteeseeeseedeveee 5 8 spares Parts c r creese n essit E 5 9 summary of procedure eee 5 3 COUCH SCLEEN ienie 5 10 installation category s es 3 20 Intensitron HCL see Lamp 06 4 8 K keyboard COMMECHON siioni e 5 24 L laboratory exhaust Vent isomeerien enote 3 12 19A AE E ees ee 3 6 reqg ireMENtS See iniscisriiseri tenier kerivsss 3 7 lamp aloin eere aN ess 6 29 ALiQNMENE ser iiinn 4 10 4 11 alignment controls sseesseeeeereeeeeseee 6 29 CICAMING eree preceito eeens 4 10 coded lamp 0 0 eeeceesteceeneeee 6 30 7 10 coded multielement lamp 6 30 COMPALtMEN eee eeeeeeeeereeeneeeeees 6 21 A A ASA oN E wh diteinien ctl tetew 7 9 deuterium lamp aligning 9 49 deuterium lamp reassem
18. 200 instrument line is self contained with its built in touch screen and burner system to perform Flame AA determinations There are three versions of the AAnalyst 200 instrument Its basic features AAnalyst 200 P N B315 0050 include a touch screen a single lamp and a burner system with automatic computer programmed flame gas control It is designed for optimized cost effective automatic flame and mercury hydride analyses The second version AAnalyst 200 P N B315 0060 has all the basic features plus it contains a built in deuterium background corrector and supports one EDL lamp The third version AAnalyst 200 P N B315 0070 features an automated lamp turret and supports two EDL lamps This chapter gives a complete description overview of the AAnalyst 200 The optional autosamplers are described later in this manual System Description AAnalyst 200 Overview Figure 4 1 The AAnalyst 200 Instrument The AAnalyst 200 Atomic Absorption Spectrometer is a double beam atomic absorption spectrometer for flame and mercury hydride analysis It is a sophisticated analytical system capable of performing automated single element determinations AAnalyst 200 User s Guide The AAnalyst 200 Spectrometer System Concept The AAnalyst 200 spectrometer from PerkinElmer is a compact benchtop flame atomic absorption spectrometer featuring e Double beam optical system optimized for maximum radiation throughput e Burner system for flame
19. 232 serial cable to the comport 1 2 3 or 4 of the computer Get Connected g x Get Connected After installing batteries or plugging in the AC adapter do one of the following Use the serial cable to connect to a COM port on the back of this desktop computer and click Next Use the USB cable to connect to the USB port on the back of this desktop computer ActiveSync will automatically detect the device connection You can also connect your mobile device using infrared IR For more information click Help lt Back Cancel Help Screen 7 29 Get Connected Window 4 From the AA application Touch Screen touch the Tools button to access the Tools dialog Do not power off the instrument or disconnect the serial cable while downloading There is a slight risk of application failure to CAUTION recover 7 42 AAnalyst 200 User s Guide New Method Save Method Sample Information Select Method Print Method Startup Options Print Results Recommended Conditions Calibrate Stylus Set Date and Time Regional Settings hey zs i Screen 7 30 Tools Dialog from the Touch Screen 5 Touch the Download button from the Tools dialog to start the download 6 Continue from the Get Connected window and click Next 7 Ifthe Partnership dialog appears select the No option button and then click Next New Partnership x Set Up
20. 25 02 B 53 26 97 25 02 B 53 33 Cancel lt Back ne gt Finish Screen 7 40 Test Import Wizard Step 2 20 In the last window of the Wizard select the desire options from the Column data format section Click Finish to complete the importing process 7 50 AAnalyst 200 User s Guide Text Import Wizard Step 3 of 3 GIFS This screen lets you select each column and set olumn data format the Data Format General General converts numeric values to numbers date C Text values to dates and all remaining values to text pace mov Do not import column skip Advanced Data preview Screen 7 41 Test Import Wizard Step 3 21 Select Save As from the File menu to save your result as an excel file 7 51 Touch Screens 7 52 Analyzing Samples AAnalyst 200 User s Guide Sequence of Operations The diagram below shows the sequence of operations that you must perform to analyze samples using the AAnalyst 200 spectrometer The pages and dialogs that you require for each step are shown a SS Lamp Flame Prepare Standards C Page 3 L Page J and Samples J i Me A Se gt O neto Oxidant Lamps Dialog Dialog J Startup and Prepare the System L gt S A N Parameters Spectrometer Page Subpage NE KG Vz Calibration ee Subpage Enter Parameters v Optimi
21. A green icon located on the lower right hand corner of the taskbar indicates successful connection 7 48 AAnalyst 200 User s Guide New Partnership s x ca Set Up a Partnership t 2 Before you can synchronize information between your mobile device and this computer you must set up a partnership between them Would you like to set up a partnership C Yes Set up a partnership so that can synchronize information between my device and this computer No don t want to synchronize information Set up my device as a quest so that can copy or move information between my device and this computer Screen 7 37 New Partnership Dialog 13 When the ActiveSync window appears on the screen click the Explore icon A window appears displaying thumbnails of files and folders stored on the AAnalyst 200 3 Microsoft ActiveSync 5 xl Fie view Tools Help e Sync Stop Detail Guest Connected Explore Options Information Type Status Screen 7 38 The Microsoft ActiveSync window shows the connection 14 Double click on My Computer and then on result directory 15 Click on the result dat and copy the file to the computer clipboard Select Copy from the Edit menu or press Crtl C 16 Within Windows Explorer paste result dat file into the desire directory Select Paste from the Edit menu or press CTRL V 7 49 Touch Screens 17 Laun
22. ER n T DESCE Ei 2 22 Electromagnetic Compatibility EMC sssssesesesseesesrrssereresresrrsresrrsrreseses 2 23 WEEE Instructions for PerkinElmer Products 000 0 cee ceeeeeceeeeeeeeeeeeeeeee 2 24 References for Laboratory Safety Practice 0 0 cece eseeseesseceseeeeeeeeeeeeeeees 2 25 Chapter 3 Preparing Your Laboratory TrtrOMU Ct ON sess ic se Sinte ss Voss eh lek e E lad a e E EE aiT 3 3 Environmental Conditions ceseessecssecsseceseceseceseceseeeseeseneeeneeeaeeeaaesaaees 3 4 General Laboratory Requirements 000 0 eee eeeeseeeseeereeeneecnseesaeceaeenseenseeees 3 5 Location and Space Requirements 20 0 0 cc cescesceseceseceseeeeeeeeeeeeseeeseeeaeeenaees 3 7 Exhaust Vent Requirement 00 0 esecseesecseceseceseceseceseceeeeseesseeeeneeeaes 3 12 Electrical Requirements sie 2 3 00s cieeceeistiechiiviiedad a E a 3 20 Camps necer eaa e Ee IE A EI EE A es svbechase sdanates A EEIN IEE 3 21 Chapter 4 System Description Introduction senn Hees te eae aa ee a 4 3 A Analyst 200 Overviewess csciet cesses ieteas iscsi A E aa ar Eee 4 4 The AAnalyst 200 Spectrometer System 0 0 0 ee eeeeeeeeeseeereeeeeeseceseenseeees 4 5 General Lamp Information sarres ninnan atei e E 4 6 The Deuterium Arc Background Corrector sseeseeeseereeeereeresreerrsrreseses 4 11 The Burner Systemerne wes lawl ie Glee ede 4 12 Connecting the Electrical Supply cee ee eeeeeseeeseeeeeeeeceaecnseeeeeeseeeeaes 4 19 Mercury Hydride Determination System MHS 15
23. Environmental Conditions e General Laboratory Requirements e Laboratory Space Requirements e Exhaust Vent Requirements e Gas Supply Requirements e Electrical Requirements e Lamps Make sure your laboratory meets all of the requirements before you begin to install the system 3 3 Preparing Your Lab Environmental Conditions The laboratory in which the AAnalyst 200 is located must meet the following conditions A corrosive free environment The instrument will operate with a laboratory temperature between 15 and 35 C 59 95 F with a maximum rate of change of 3 C 5 F per hour The environment should be relatively dust free to avoid sample and instrument contamination problems Free of excessive vibration Free of direct sunlight The relative humidity should be between 20 and 80 noncondensing Two types of flames are commonly used for atomic absorption flame analysis air acetylene or nitrous oxide acetylene Air acetylene is the preferred flame for the determination of about 35 elements by atomic absorption The temperature of the air acetylene flame is approximately 2300 C 4200 F For most air acetylene flames the acetylene flow used is about 4 liters per minute or 0 14 cubic feet min Using a heat combustion value of 1 450 BTU per cubic foot the heat given off would be approximately 12 300 BTU per hour The nitrous oxide acetylene flame has a maximum temperature of approximately 2800 C 5100 F
24. For setup amp optimum performance warm HCLs for 5 10 minutes and 30 minutes for EDLs Repeat the lamp procedure Coded single element Lumina lamp 1 2 Start up the spectrometer but do not ignite the flame Lamps Installed are automatically shown in the energy display box on the Lamp page The element entry field box automatically shows the element installed Touch the Setup Instrument button on the Lamp page of the touch screen The recommended parameters for that element are automatically set up e The system automatically switches the lamp on sets up the optical path prism and grating sets and peaks the wavelength sets the slit and performs an Automatic Gain Control AGC and Automatic Intensity Control AIC Turn the two alignment controls alternately and in small increments while watching the AA bar graph and the numerical energy display Align the lamp to obtain maximum energy Coded single multi element Lumina lamp 1 2 Unc 1 2 6 30 Start up the spectrometer but do not ignite the flame Lamps Installed are automatically shown in the energy field box on the Lamp page The element entry field box automatically shows the element installed Touch the Element entry field box on the Lamp page to display the Select Element dialog You select the desired analyte element from the list in the dialog Touch the OK button and the recommended parameters for that element are automatically set up Tu
25. Full Name Description Password and password options New user hl User name User Full name Users Description High ccess User Password Confirm password mo O O JV User must change password at next logon J User cannot change password Password never expires I Account is disabled oe Screen 7 26 New User dialog NOTE It is suggested that the User must change password at next logon is selected as the password option This will allow the User s password to be unknown to anyone other than that User It is also important to provide the full name of each user The Enhanced Security software uses the full name to identify the user in all of its logging features e Double click on UserA A Properties dialog appears for UserA e Click on the Member Of tab and then add UserA to the desired group using the Add button We will add UserA to the Administrators Group We also need to add UserA to the Users Group Click OK 7 38 AAnalyst 200 User s Guide To set permissions for the AA200 Result Data directory From the C directory right mouse click on the AA200 Result Data folder Select Properties Click on the Security Tab Deselect Allow inheritable permissions from parent to propagate to this object 44200 Result Data Properties Gi ks General Sharing Security Name Add gi Administrators Remove Permissions Allow Deny Full Control Modify Read amp Execut
26. To analyze the sample indicated by the sample number entry field box touch this button A green light appears on the button when selected To display the calibration curve window touch this button Touch this button to resize the graph of the most recent or current absorbance reading By default the print function is On and the results will print when the printer queue is full The green light indicates that it is On To turn print function Off touch Printer On Off button This will print any results in the printer queue Entry Fields on Analyze page Standard Concentration Sample Number ID Number Box Dilution Box 7 24 Touch this entry field box to view the standard concentration dialog Use the dialog to select the standard concentration you want to analyze The standard concentration will automatically increment after each standard run A calibration curve is created after all blanks and selected standards are run This entry field box shows the sample number of the sample you are currently analyzing If you wish to analyze a different sample touch this entry field box to view the sample number dialog The sampler number will automatically increment after each sample run This entry field allows you to enter the ID number for the sample This entry field allows you to enter the sample dilution AAnalyst 200 User s Guide Analyze Page Autosampler This window allows users to setup and perform automated ana
27. a Partnership ap t Before you can synchronize information between your mobile device and this computer you must set up a partnership between them Would you like to set up a partnership C Yes Set up a partnership so that can synchronize information between my device and this computer No don t want to synchronize information Set up my device as a quest so that can copy or move information between my device and this computer lt Back Cancel Help Screen 7 31 New Partnership Dialog 7 43 Touch Screens 8 The Microsoft ActiveSync window appears and displays the status of the connections between the E Box and the computer NOTE A green icon located on the lower right hand corner of the taskbar indicates successful connection 3 Microsoft ActiveSync loj xj File view Tools Help BS amp Sync Stop Details Explore Options Guest Connected Information Type Status Screen 7 32 The Microsoft ActiveSync window shows the connection 9 Connection is established Downloading Once the connection is established between the computer and the E Box continue with the procedure below for downloading 1 Insert the QuickStart CD 0993 6637 into the computer and use the browser to find Update bat file 2 Double click on the Update bat 3 The command prompt window appears and the download of the software firmware to the E Box begins
28. a predetermined shutdown sequence to extinguish the flame safely 4 Shut down the gases to the spectrometer at source 5 Touch the Bleed Gases button to depressurize the gas lines 9 12 NOTE NOTE AAnalyst 200 User s Guide Cleaning the Burner Chamber Do not scrape the plastic components with metal tools Do not soak the burner chamber in acid or use abrasive cleaner 1 4 5 Remove the burner system from the atomizer compartment and take the burner chamber apart Clean the burner chamber and flow spoiler with a soft brush and a mild laboratory detergent solution Clean the inside of the burner end cap with a soft brush and a mild laboratory detergent solution After cleaning rinse thoroughly with deionized water Reassemble the burner system Cleaning the burner chamber after use with organic solvents If you aspirate aqueous samples immediately after organic samples e g oils or MIBK extracts the absorption signals can be noisy and erratic After aspirating organic samples perform the procedure below to prevent contamination of subsequent aqueous samples 1 Aspirate for 5 minutes an organic solvent that is miscible with the samples that have just been aspirated Aspirate methanol or another solvent miscible with both the organic solvent and water for 5 minutes Aspirate 1 nitric acid solution for 5 minutes Flush the drain tube thoroughly with water Empty the collection vessel and refil
29. and blank Rerun proven standards Change blank Cannot get close to suggested characteristic concentration Possible Cause of Problem The flame may have been too rich or too lean for the element being determined You may not be comparing the characteristic concentration specified for the wavelength you are using The instrument may not be using the correct wavelength If the element is easily ionized ionization suppressant may be required The fuel and oxidant flows may not be set properly or the wrong type of flame may be being used Slit width may be too wide Nebulizer may not be adjusted properly AAnalyst 200 User s Guide Check and or Remedy Refer to the recommended flame conditions in the Standard Conditions window for the element or the Analytical Methods manual Recheck the characteristic concentration for the wavelength Check the wavelength If a problem is found contact a PerkinElmer service engineer for assistance Add approximately 1000 mg L of an easily ionized salt such as potassium lithium or lanthanum to samples standards and blank Adjust the gas flows or change to a nitrous oxide acetylene flame if appropriate Check recommended settings in the Standard Conditions window for the element being determined Adjust the nebulizer using the information given in this User s Guide 10 5 Troubleshooting Cannot get close to suggested characteristic concent
30. and is also used for the determination of elements which form refractory oxides It is also used to overcome chemical interferences that may occur in flames of lower temperatures For the nitrous oxide acetylene flame the acetylene flow is about 14 liters min or 0 5 cubic feet per min Using a heat of combustion value of 1 450 BTU per cubic foot the heat given off would be approximately 43 000 BTU per hour AAnalyst 200 User s Guide General Laboratory Requirements Operating conditions Warning Explosive Atmosphere This instrument is not designed for operation in an explosive atmosphere WARNING Recommended operating conditions e _ Indoors The location must be free of smoke dust corrosive fumes direct sunlight and excessive vibration e Temperature 15 C to 35 C 59 F to 95 F Maximum rate of change not exceeding 3 C 5 F per hour e Relative humidity 20 to 80 without condensation e Altitude in the range 0 m to 2 000 m sea level to 6562 feet Safe operating conditions e Indoor e Temperature 5 C to 40 C 41 F to 104 F e Relative humidity 20 to 80 without condensation e Altitude in the range 0 m to 2 000 m sea level to 6562 feet Storage conditions e Ambient temperature 20 C to 60 C 4 F to 140 F e Relative humidity 20 to 80 without condensation e Altitude in the range 0 m to 12 000 m sea level to 39 370 feet 3 5 N
31. atmosphere especially near the ceiling e Never allow the outlet gauge pressure to exceed 103 kPa 1 03 bar 15 psig acetylene can explode spontaneously above this pressure e Prevent acetylene from coming into contact with copper silver mercury or gaseous chlorine e Solvent carryover If the acetylene cylinder pressure falls to below 600 kPa 6 0 bar 87 psig at 20 C some of the solvent used to stabilize the acetylene such as acetone may be carried over into the burner This could influence the characteristics of the burner with a resulting influence on the analytical results Change to a new acetylene cylinder when the cylinder pressure falls below this value 3 19 NOTE Preparing Your Lab Electrical Requirements The following section describes the power requirements for all the components that make up the AAnalyst 200 system The AAnalyst 200 spectrometer requires a stable single phase electrical supply of 100 230 VAC 10 50 Hz or 60 Hz 1 capable of providing 300VA maximum that has a correctly wired protective earthing system ground connection The line power supply should be free of line transients in excess of 50 V peak If the electrical supply voltage produces large AC line voltage fluctuations a qualified electrician should install a voltage regulator between the electrical outlet and the instrument The line power supply point must be within 2 meters of the rear of the spectrometer We rec
32. be used at wavelengths below 230 nanometers nm or a UV transmitting glass window for lamps to be used at longer wavelengths The cathode is a hollow cylinder of the metal whose spectrum is to be produced Both the anode and cathode are sealed in the glass cylinder The quartz graded seal or glass window is fused to the glass cylinder 1 Sputtering 2 Excitation 3 Emission Anode Window y Art Art gt a o Z AF yo Me M gt M Cathode Fill Gas Figure 4 2 The workings of a hollow cathode lamp HCL AAnalyst 200 User s Guide Hollow cathode lamps emit light by the following process the fill gas is ionized when an electrical potential is applied between the anode and the cathode The positively charged ions collide with the negatively charged cathode and dislodge individual metal atoms in a process known as sputtering These sputtered metal atoms are excited through impact with fill gas ions Light of the specific wavelengths for that element is emitted when the atom decays from the excited state to a more stable state Lumina Hollow Cathode Lamps The Lumina hollow cathode lamps were designed for use with the AAnalyst series of atomic absorption spectrometers They are the latest innovation in optimizing light sources for AA spectrometers These lamps provide fully automated wavelength current and slit selection which results in reduced setup times for easy and accurate operation Lumina Hollow Catho
33. bottom bracket Figure 9 2 Removing the burner door 1 Swing the door open to about the 45 position 2 Exert enough upward pressure on the lower left corner of the door to tilt the top of the door away from the upper door bracket 3 Lower the door free if the bottom bracket Removal is complete 9 15 Maintenance Replacing the Burner Door Refer to the figure below when re installing the burner door Burner sal f 1 Figure 9 3 Replacing the burner door 1 Hold the door in place next to the burner compartment as shown in the figure above 2 Tilt the top of the door away from the upper door pin while you push the lower pin into the hole in the door mount 3 Drop the top pin down into the upper hole in the door mount while holding the bottom pin in place Swing the door while letting it drop down and lock into place on the hinges 4 Close the door Re installation is complete 9 16 AAnalyst 200 User s Guide Cleaning the Burner System The nature of the samples aspirated determines how frequently you need to clean the burner system e The burner should provide an even flame over the length of the burner slot An uneven flame may indicate that the slot needs cleaning A badly clogged slot may cause a flashback of the flame e Aspirating samples with high solids content may cause deposits to build up along the burner slot e Pro
34. correctly installed and connected to their AC line power outlets 2 Ifyou need the optional autosampler connect the autosampler to AC line power 3 Switch on the exhaust venting system for the work area 4 Turn on the burner gases and adjust the outlet gauge pressures to the recommended values Always set the same outlet gauge pressure for air and nitrous oxide 5 Install the required lamp for the analyte element 6 Switch on the spectrometer using the AC power on off switch located on the E Box 7 Set up the burner system 8 Procedures for shutting down the system are described in Chapter 8 Analyzing Samples In an emergency you can shut down the system as described in Chapter 8 Analyzing Samples Required Pressures for the Burner Gases Purge Air C2H2 eal line black line red line ma Pe seat et m Pa a a bar oo 4o ao so ao ao foe fio psu u ls ae s u so ro Ji e Set the outlet gauge pressure for each gas to a value just below the maximum value P max e Always set the same outlet gauge pressure for air and nitrous oxide e Never set the outlet gauge pressure to a value exceeding the maximum pressure Pmax Operation of the Instrument e Only high quality purge gases Air Ar or N2 should be used Minimum purity of 99 9 is recommended A high quality filter dryer accessory is recommended for the removal of any moisture from the purge gas Warning Acetylene Explosion Hazard Acetylene can
35. cylinders vertically rather than horizontally to prevent liquid acetone form reaching the cylinder valve The practice of cracking the valve of an acetylene tank that is opening the valve slightly for a very short period previous to attaching the regulator is not recommended While such an action will clear the valve opening of dust or dirt particles and may remove acetone from the cylinder valve it is a potentially hazardous practice and one which should never be attempted in the presence of an open flame sparks or other possible sources of ignition 9 50 AAnalyst 200 User s Guide Replacing the Lamps Always wear UV absorbing safety glasses when installing replacing or aligning hollow cathode lamps or electodeless discharge lamps The ultraviolet radiation emitted by these lamps can harm your eyes WARNING Lamp Compartment Location The next figure shows where the lamp compartment is located on the instrument Access to the lamp compartment is at the front of the spectrometer This allows for easy lamp replacement If you swing open the lamp compartment cover it is the door below the Touch Screen the lamp compartment can be seen inside Figure 9 17 Accessing the lamp compartment 9 51 Maintenance Replacing the Deuterium Arc Background Corrector Lamp Since the instrument cover will be removed this procedure should be done by a Skilled person who is trained in the servicing of optic
36. described in the User s Guide provided with the autosampler Set up the autosampler by following the directions given in Chapter 6 Operation of the Instrument Load the autosampler In the autosampler tray location zero 0 is reserved for the wash 1 is for blank and locations 2 through 9 are reserved for standard solutions The last standard location is reserved for reslope If not already done load the autosampler tray with a blank standards and samples Enter parameters Refer to Chapter Touch Screen section Analyze Page Autosampler if you require information on how to enter analytical parameters Fill in the entries for autosampler tray first and last sample location and recalibration frequency If not already done install and align the required lamp and ignite the flame On Parameters page Spectrometer subpage 1 Enter 1 second for the Integration Time 2 Enter 3 for the number of Replicates 3 Enter 3 seconds for the Read Delay 4 Enter the required Print parameters 8 17 Analyzing Samples 5 Select the information you would like to have printed together with the analytical results 6 Select Autosampler for Sample Handling N R I n IN N TN IN A m a T T IN IN IX I n D R Screen 8 9 Parameters page Spectrometer subpage On Parameters page Calibration subpage 1 Select the Calibration Equation 2 For this example select Linear Through Zero Enter mg L for
37. flame if the drain system is not functioning properly If the liquid level in the trap is too low the switch is activated and the flame is shut down 4 16 AAnalyst 200 User s Guide me D spiral Wrap Drain Interlock Cable r 3i Connector at Burner i oO Y Interlock Cable X i i Drain Tubing Retainer Cap Drain interlock Float Switch Assembly Waste Vessel Figure 4 10 The burner drain system and its parts Burner Installation The entire installation of the burner is covered in Chapter 6 Operation of this User s Guide Manual The basic steps are bulleted below for your reference Directions on how to perform each step are discussed in detail during installation e installing the nebulizer on the burner e checking that the burner end cap is secure e connecting and securing the gas hoses to the burner e installing and securing the burner head 4 17 System Description e installing the quick change burner mount assembly into the instrument e installing and connecting the burner drain system Burner System Maintenance Refer Chapter 9 Maintenance in this User s Guide manual for extensive burner system maintenance information Burner System Troubleshooting We recommend that you consult the troubleshooting information included in this manual before you call a PerkinElmer service engineer Refer to Chapter 10 T
38. hand tight plus a 4 turn using two wrenches one wrench to hold the nebulizer fitting and the other to turn the compression fitting Operation of the Instrument Installing and Securing the Burner Head The burner head is shipped from the factory already attached to the burner assembly 10 cm air acetylene N040 0102 If it was removed or you need to change it follow these instructions to put it back on Make sure the magnetic strip is facing the ignitor box You must also confirm that the burner head safety latch is positioned above the head ring This procedure will make sure that safety latch is correctly positioned over the burner head ring gt Safety Latch a Bumer Hoad corectly positioned _ Bumer Head Ring over Burner Head Ring Magnetic Strip around back ignitor can swing Fa over Burner Burner Head gia in place Chamber _ lgnitor Box fe Safety Latch ey _ _ O Ring Figure 6 5 Confirm that the burner head is in place and latched securely 1 Press the tab on the safety latch while lowering the burner head into place inside the o ring see figure above 2 Confirm that the magnetic strip on the burner head ring is positioned around back and facing the ignitor box See the left most drawing above 3 Make sure to completely seat the burner head onto the chamber by gently pushing and twisting the burner head into the chamber See the right most drawing above
39. head cools down 2 To remove and install the burner head refer to chapter 9 Maintenance 3 On the Flame page touch the Oxidant entry field box Select the oxidant type from the Oxidant dialog Screen 7 7 Oxidant dialog NOTE Ifan air burner head is installed the Nitrous oxide option is automatically grayed out 7 11 Touch Screens Continuous Graphics Window on the Flame page The Continuous Graphics window contains a continuous real time plot of absorbance or emission against time The scale for Y axis and real time absorbance default value ranges from 0 00 4 00 absorbance Parameters on Flame page Oxidant Touch entry field that displays the selected oxidant acetylene or nitrous oxide To select or change the oxidant touch this field to display the oxidant dialog Select the required oxidant in this dialog If you select nitrous oxide as the oxidant the flame will be ignited with an air acetylene mixture with automatic changeover to nitrous oxide after a few seconds Oxidant Flow Touch entry field with associated arrow keys that L min displays the selected oxidant flow rate in liters min To change the flow rate you can either e Touch the field to display the Oxidant Flow dialog and enter the required flow rate in this dialog or e Touch the increase or decrease lt 4 arrows the flow rate is changed in increments of 0 4 L min Acetylene Flow Touch entry field with associated arrow
40. heated to dissociate the hydride gas into free atoms or in the case of mercury to prevent condensation of the water vapor Plunger Reaction Flask Socket BD Bayonet Lock lt __ Reaction Flask Figure 4 12 The MHS 15 and its parts 4 21 System Description The MHS 15 is a manual system The quartz cell is heated by the flame Key operating parameters are controlled by the instrument touch screen Data collection calibration and calculation functions are performed by the instrument The MHS 15 analyzer assembly is freestanding and is located near the sample compartment of the spectrometer This assembly includes a reaction flask a reservoir for the reducing agent and all pneumatic components for control of the carrier gas and transport of metallic vapors to the quartz cell The cell assembly consists of a quartz cell and a mount The mount installs on the AAnalyst burner head positioned above the single slot in the burner head permitting the quartz cell to be heated in the flame Sample Inlet i N Quartz LA Cell i a LV f Transfer Hose i I 4 Burner G Head Burner Chamber Figure 4 13 The MHS 15 sample cell mounted on the burner For detailed information on the MHS 15 refer to the manual that came with the System 4 22 Installation 5 NOTE AAnalyst 200 User s Guide Introduction to the Installation Procedure Before you start to install your AAnalyst 200 spectrom
41. if the beams are not coincident the same centers tweak the alignment screws to center the Hollow Cathode Lamp beam inside the deuterium arc lamp beam The next figure illustrates the ideal appearance of the two beams 9 54 AAnalyst 200 User s Guide Hollow Cathode Lamp Beam Orange Deuterium Arc White Card Lamp Beam Violet Burner Slot Burner Head Figure 9 20 The centering of the two lamp beams The alignment procedure is now complete 9 55 Maintenance AS 90plus and AS 93plus Autosampler Maintenance Routine Maintenance Minimal routine maintenance is required Keep the carousel clean and try to avoid spills Do not use abrasives to clean the clear plastic carousel cover Do not use organic solvents to clean the carousel cover For more information refer to the manuals received with the Autosamplers For the AS 90plus Autosampler see manual B314 0291 and for the AS 93plus Autosampler see manual B314 0330 Spare Parts If corrosive solutions are being routinely analyzed a corrosion resistant platinum rhodium probe is available to replace the standard stainless steel version on the AS 90plus and AS 93plus Autosamplers You may find it convenient to purchase additional sample trays so that samples may be loaded into a second carousel while the first is still in use For spare parts refer to the AS90 or AS93 manuals provided with the Autosamplers or the e ssentials catalog Servicing Se
42. indicate that the lamp is starting to deteriorate As a hollow cathode lamp reaches the end of its useful life the current on the lamp may be increased up to the maximum current recommended on the label Once the intensity of a lamp begins to deteriorate it should be replaced Lamp Troubleshooting Refer to Chapter 10 Troubleshooting in this manual for lamp troubleshooting information To avoid damages to the instrument do not insert EDL s or non linear lamps too far into the lamp holder CAUTION 4 10 AAnalyst 200 User s Guide The Deuterium Arc Background Corrector An Explanation The Deuterium Arc Background Corrector The Deuterium Arc Background Corrector is an internally mounted assembly that provides correction for molecular absorption and light scattering The spectrometer uses a deuterium arc lamp to correct for background absorbance caused by non atomic species in the atom cloud When the deuterium arc background corrector is used two alternating sets of measurements are made one with the primary source and a second with the background corrector source The primary source measures a combination of background and atomic absorption The continuum source measures only the background The difference between the two measurements yields the atomic absorption A deuterium arc source is used for maximum wavelength coverage and intensity The AAnalyst can accurately handle combined atomic plus background absorption sign
43. keys that L min displays the selected acetylene flow rate in liters min To change the flow rate you can either e touch the field to display the Acetylene Flow dialog and enter the required flow rate in this dialog or e touch the increase or decrease lt 4 arrows the flow rate is changed in increments of 0 2 L min 7 12 AAnalyst 200 User s Guide Buttons on Flame page Flame On Off Touch the On side of this switch to ignite the flame Touch the Off side of this switch to extinguish the flame In an emergency press the Red Emergency button located on the upper left side of the instrument The system will extinguish the flame Bleed Gases After extinguishing the flame and shutting down the gases at source touch this button to depressurize the gas lines Auto Scale Graph Touch this button to resize the graph of the most recent or current absorbance reading Auto Zero Graph Touch this button to set the reading for the current signal to zero on the graph Interlocks The burner system has a safety feature that monitors gas pressure and checks for proper setup of the burner head nebulizer and drain system A green check mark shows that all safety interlocks are satisfied and that you can ignite the flame A red cross mark indicates an unsatisfied safety interlock You must correct the hardware condition causing the problem before attempting to ignite the flame Touch the interlock field box to v
44. lamps that are required See chapter 6 for Aligning Lamps Follow the procedures for setting up Flame Analyses including setting up and adjusting the burner and igniting the flame in chapter 6 Once you are ready to perform the analysis see the procedures for Manual Flame Analyses in this chapter NOTE To initiate the read touch the Analyze Samples button on the Analyze page Wait for the specified BOC time to elapse typically 2 seconds then press the plunger down on the MHS 15 8 22 AAnalyst 200 User s Guide Running Samples in Emission Mode The AAnalyst 200 also performs flame emission measurements at a fixed wavelength This option is useful when you do not have a lamp for the element you wish to determine or if you are determining elements such as Na K Ca or Ba which are sensitively determined by emission A setup solution containing the element being determined must be aspirated while the spectrometer wavelength is peaked and the high voltage gain on the photomultiplier is set For each element the concentration of the setup solution should be the same as the concentration of the highest calibration standard Aspirating the setup solution produces an emission signal that is required to peak the wavelength for the maximum signal and to set the photomultiplier voltage to the proper value Setting Up for Emission Refer to the section on Standard Conditions in Analytical Methods for Atomic Absorption Spectrometry
45. meets all of the requirements listed in Chapter 2 before you begin to install the system Fittings suitable for most commonly available gas regulators are provided in the installation kit supplied with the spectrometer Air and nitrous oxide fittings have right hand threads Acetylene fittings have left hand threads Gas hoses on the spectrometer Warning Flammable Gases Fire and Explosion Hazard Acetylene is a flammable gas Make sure that all the gas connections are gas tight Check the connections and gas hoses regularly for leaks using a leak testing fluid WARNING Gas Pressures Gas Purge N O Air C H clear line black line red line min max min max min max min max kPa 300 400 300 400 300 400 80 96 bar 3 0 4 0 3 0 4 0 3 0 4 0 0 8 1 0 psig 44 58 44 58 44 58 12 14 1 Connect the purge clear air black nitrous oxide blue and acetylene red hoses to the respective gas supplies Fittings suitable for most commonly available gas regulators are provided in the installation kit supplied with the instrument 2 Tighten all gas connections using the double wrench technique hold the fitting on the regulator with one wrench and tighten the compression nut on the gas hose with the other wrench Acetylene fittings have left hand threads Air and nitrous oxide fittings have right hand threads 3 Only high quality purge gases Air Ar or N2 should be used Minimum purity of 9
46. order e N040 0100 5 cm single slot burner head for nitrous oxide acetylene operation e N040 0101 5 cm single slot burner head for air acetylene operation It features a wider slot than the nitrous oxide burner head e N040 0102 10 cm single slot burner head for air acetylene operation standard with all burners e N040 0103 10 cm three slot burner head for analysis of high dissolved solids content solutions with air acetylene flames The 5 cm single slot air acetylene burner head is rotatable to 90 degrees N0O40 0100 5 cm 2 in NO40 0101 5 cm 2 in Nitrous Oxide Operation Air Acetylene Operation L Positioning ZL eo Notches 45 N H magneti 4 A idenifeation X L Strip Z N040 0102 10 cm 4 in N040 0103 10 cm 4 in Air Acetylene Operation 3 Slot Air Acetylene Operation J 7 g Figure 4 9 The four available burner heads 4 15 NOTE System Description The Burner Mount The quick change burner mount provides horizontal vertical and rotational adjustment The quick disconnect release lever simplifies removal of the burner assembly The Ignitor Assembly The ignitor assembly includes the glow plug the ignitor solenoid and ignitor arm the burner head interface circuit and the flame detect circuit When the ignitor is activated automatically the glow plug is energized and heats up The ignitor solenoid which is also energized swings the ignitor arm into pl
47. procedure for powering up the spectrometer is described in Chapter 6 Operation of the Instrument 5 23 Installation Switches and Connectors on the E Box All electronics are located in a single user replaceable module called the E Box Switches and connector ports are located on the front panel of the E Box as shown in the figure below Autosampler Serial 1 Ethernet Remote Trigger EDL 1 EDL 2 Printer Keyboard Display On Off Switch AC Input 5 24 Remote Trigger Printer EDL2 EDL1 Ethernet Autosampler Keyboard Display AC Input On Off switch Figure 5 12 Switches and ports on the front panel of the E Box Connection port for autosampler Connection for serial port Connection port for the network Connection port for foot switch or FIAS Read cable Connection port for EDL in lamp position 1 Connection port for EDL in lamp position 2 Connection port for printer Connection port for keyboard Connection port for the touch screen Power switch Connection of the power line cord AAnalyst 200 User s Guide Setting Up the AutoSampler The AA200 Analyst supports autosampler model AS 90 AS 90 plus p n B314 0291 and AS 93 plus p n B314 0330 Depending on your autosampler model refer to the User s Guide provided with your autosampler for complete installation Electrical connections Connecting autosampler AS 90 plus or AS 93 plus to the E Box 1 Connect RS 232 cable to
48. proprietary leak testing fluid Call a PerkinElmer service engineer if a leak is detected Acetylene cylinder If the cylinder pressure falls to below 600kPa 6bar 85 psig some of the solvent sed to stabilize the acetylene e g acetone may be carried over into the burner This ould influence the characteristics of the burner Always change to a new acetylene ylinder when the cylinder pressure falls to below this value Maintenance Warning Unauthorized Adjustments and Servicing Only a PerkinElmer service engineer or similarly trained and authorized person should be permitted to service the instrument WARNING If the spectrometer system does not function correctly e Switch off the spectrometer system and make sure that it cannot be operated e Contact your local PerkinElmer office You should only perform the maintenance procedures described in this guide For any other maintenance or service contact your local PerkinElmer office to arrange for a service engineer to visit In particular you should only allow a PerkinElmer service engineer or similarly trained and authorized person to perform any work on 1 Electrical components inside the instrument excluding the E Box 2 The gas connections and gas system pneumatics 3 The monochromator and all other optical system components Before the service engineer arrives e Make sure that the instrument and work area are clean e Empty corrosive solutions from the burner drain ves
49. regulator to give the maximum absorbance reading NOTE You should not need to move the adjusting nut very much to obtain the maximum reading if the nebulizer was correctly preadjusted 6 40 AAnalyst 200 User s Guide Optimizing the gas flows The oxidant to fuel ratio affects the sensitivity of the analyses although the magnitude of the effect varies between elements Generally you adjust the gas flow rates to give maximum absorbance for the analyte element Some elements require an oxidizing air acetylene flame blue fuel lean hot and some require a reducing flame yellow fuel rich and relatively cool 6 41 NOTE Operation of the Instrument There are two ways to alter the gas flow rates while you are performing the optimization procedure e Touch the flow field to display the Flow dialog and then enter the required flow rate in this dialog or e Touch the increase gt or decrease 4 arrows The system checks that the flow rate values you have entered are within the safe working range Optimization procedure 1 Touch the Flame tab to display the Flame page 2 Aspirate the blank solution and when the signal is steady touch the Auto Zero Graph button 3 Aspirate the standard solution 4 Initially adjust the fuel and oxidant flow rates to obtain the type of flame given in the Recommended Conditions 5 Then make incremental changes to the fuel and oxidant flow rates alternately while at the same time
50. remove the burner head press the tab on the safety latch found on the ignitor box At the same time gently pull and twist the burner head in an upward direction until it comes off the chamber right most drawing below Safety Latch positioned above Burner Head Ring Lift Bumer Head ignitor Box away from Chamber Ignitor must be off to the side i I i I I I U Bumer Head Chamber Figure 9 4 Removing the burner head from the burner chamber 9 22 AAnalyst 200 User s Guide Removing the Burner Assembly from the Instrument 1 Extinguish the flame turn off the gases and power down the instrument Let the burner head cool Open the burner door 2 Disconnect the drain tube unplug the drain interlock connector 3 Locate the locking pin on the burner assembly and pull upward to unlock the lever Locking Pin Lever Figure 9 5 Burner side view 4 Push the lever forward to release the burner assembly 5 Slide the assembly out and place the burner assembly on a bench 6 The assembly is now ready for servicing 9 23 Maintenance Locking Pin Figure 9 6 Removing the burner assembly from the instrument 9 24 AAnalyst 200 User s Guide Disassembling the Burner Chamber These procedures assume that you have removed the burner assembly from the instrument and placed it on a workbench Next you will disassemble it 1 Press the safety latch tab on the ignitor box whil
51. the drain outlet on the burner end cap Tighten the clamp securely Place the other drain clamp on the lower end of the drain tubing Then attach the tubing to the drain trap switch assembly Tighten the clamp securely Plug the drain interlock connector into the receptacle under the burner Make sure the interlock connector is plugged in all the way 10 Go to Preparing the New Drain Tubing for Use next Preparing the New Drain Tubing for Use This important procedure MUST be performed at this point of the drain tube replacement process In order for the sample introduction system to drain smoothly the internal surface of the new drain tube needs to be prepared This is easily accomplished when you 1 Aspirate a 50 50 solution of water and methanol for approximately 5 minutes 2 Replacement and preparation is now complete 9 34 AAnalyst 200 User s Guide __ Drain Tubing N J a Interlock Cable Vy Spiral Wrap CD NMA Retainer Cap _ Drain Trap es VAS Assembly A f Se Drain Loop KE Figure 9 12 The drain trap assembly Adding Water to the Drain Float Assembly Enough water must be present in the drain system to fill the drain loop and to activate the drain float assembly If not carry out the following procedure 1 Loosen the drain clamp and remove the drain tubing from the drain outlet on the burner end cap 2 Pour about 250 mL
52. the Autosampler connector on the E Box 2 From the E Box run the RS 232 cable to the com port 2 of the autosampler 3 Plug the autosampler power cord to the power outlet and power up the autosampler Your autosampler electrical connections are now complete For complete procedure on how to select autosampler type see Chapter 7 Touch Screens Autosampler os Hie IOc sO RS 232 Cable Autosampler OOS him 5s Figure 5 13 Autosampler Connection 5 25 Installation Connecting the Foot Switch The AA200 Analyst supports the foot switch p n 0999 8306 The foot switch is an optional feature that allows the user to conveniently analyze samples without touching the analyze button on the touchscreen The user simply steps on the foot switch and starts analyzing sample Electrical connections Connecting foot switch p n 0999 8306 to the E Box 1 Connect the foot switch connector cord to the Remote Trigger port on the E Box see figure below 2 Your foot switch electrical connections are now complete Remote Trigger E Box Foot Switch lt Figure 5 14 Foot Switch 5 26 Operation of the Instrument AAnalyst 200 User s Guide Starting up the System Summary of the procedure Read the safety information at the front of this guide before you operate the system 1 Make sure that the spectrometer system and other ancillary instruments are
53. the blue Tools button located on the bottom of the touchscreen This dialog is a collection of function and utility buttons New Method l Save Method Sample Information Select Method Print Method Startup Options Diagnostics Print Results Recommended Conditions Network Calibrate Stylus Set Date and Time Regional Settings Download Service Optical Position Screen 7 16 Tools Dialog Buttons on Tools Select Method Touch this button to open a dialog of stored methods A stored method can be retrieved by selecting the name of the method Save Method Touch this button to store methods Use the touch keyboard to enter the name and description of your method in this pop up dialog Sample Information Touch this button in enter sample information See the following section Buttons on Sample Information for the details New Method Touch this button to create a new method this will clear the current active method NOTE The current active method should be saved before touching this button Options Touch this button to view the options dialog This dialog allows the users to select languages autosampler model printers and to set beep function on or off 7 27 Touch Screens Diagnostics Recommended Conditions Network Calibrate Stylus Print Method Service Download Set Date and Time Regional Setting Startup Optical pos
54. the lamp door and install the touch screen Remove the lamp door 1 Loosen the lower securing screw with a screwdriver and place in a secure place Gently push out the upper part of the door from the upper pin and maneuver the lower part of the door out from the instrument Keep the screw for when you remount the lamp door 2 Lift out the lamp door and put it in a secure location 5 10 AAnalyst 200 User s Guide Install the touch screen Figure 5 4 Installing the touch screen Locate the touch screen packed separately 1 Thread the connector cord through the slot above the lamp compartment r Screen 5 1 Slot above the lamp compartment 5 11 Installation 2 Slide the touch screen over the slot in the instrument cover and gently move into place Screen 5 2 Mounting the touch screen 3 Locate the screw above the lamp compartment and tighten it Screen 5 3 Screw above the lamp compartment 4 Thread the connector cord into the channel Screen 5 4 Cable Channel 5 12 AAnalyst 200 User s Guide 5 Connect the display cable to the E Box s Display Connector receptacle E Box Display Connector Screen 5 5 E Box 6 Remount the lamp door This completes installation of the touch screen You must calibrate the touch screen when you put the spectrometer into operation for the first time 5 13 Installation Connecting the Gas Hoses Make sure your laboratory
55. the slot width The table below specifies the correct slot width and the feeler gauge required for checking 9 19 Maintenance Table 9 1 Slot Width and Feeler Gauge Slot Width Tolerance Feeler Gauge for check 0 65 mm 0 075 0 025 mm 0 7 mm 0 026 inch 0 003 0 001 inch 0 030 inch 0 5 mm 0 025 mm 0 020 inch 0 001 inch To check the slot width 1 Carefully slide the specified feeler gauge through the length of the burner slot 2 The gauge must fit tightly in the slot 3 If the gauge is loose in the slot the slot is too wide Then discard the burner head and use a new one Burner head surface The condition of the top surface of the burner head along the slot influences the stability of the signals Discard the burner head if the top surface is corroded 9 20 AAnalyst 200 User s Guide Pre Conditioning a New Burner or Drain Tube NOTE This is important procedure MUST be performed when a new burner or drain tubing is installed This procedure should be done directly after installation of a new burner and repeated if the drain tube or any of the sample introduction system components are replaced In order for a new sample introduction system to aspirate sample and drain smoothly all the internal surfaces need to be prepared This is easily accomplished by aspirating a 50 50 solution of water and methanol for approximately 5 minutes 9 21 Maintenance Removing the Burner Head To
56. weak The optics may require cleaning Burner may be contaminated Noise may be due to a highly absorbing flame in far ultraviolet range Noise may be due to a weak lamp coupled with a highly absorbing flame Noise may also be due to acetone carryover from the acetylene supply Background corrector source lamp may need replacement or alignment AAnalyst 200 User s Guide Check and or Remedy Use the most sensitive wavelength listed in the Recommended Conditions window for the element being determined Increase lamp current or replace lamp Replace lamp or increase the lamp current Or try using the next widest slit setting Although this may affect sensitivity Contact a PerkinElmer service representative Clean the burner head and burner chamber as described in the Maintenance chapter Check for proper drainage Use background correction or vary the gas flows to minimize flame absorption or maximize flame stability increase the lamp current to the max rating replace the lamp use the next widest slit setting although this may affect the sensitivity select a different wavelength or separate analyte element from a highly emissive matrix by chemical means Check the acetylene cylinder pressure For more information refer to the User s Guide Refer to the troubleshooting information on the deuterium arc background corrector later in this chapter 10 7 Troubleshooting Flame Burner Tr
57. 2 20 3 6 cleaning lamps ienna eena eer baht 4 10 compressed gases eeceeeeeceeseeceeeeeeeeees 2 14 I 4 connection displaye cieiesieutes hontai Moh ected 5 24 EDE Ad ecceitesaptetetetord sleeavehiitedecthladoateheiss 5 24 EDE Z eann aeaa 5 24 electrical supply 0 0 0 cee eeeeeeeeeeeeeeees 4 19 Cthemet xii seas onean deaiiae 5 24 foot switch oo eeeeeeeeeeeeeeeee ee 5 24 5 26 KS yDOALG a lt fieetsecFesassetchihscecattet iestests dls 5 24 power entry module eee 5 24 POWEF SWItCH on eee ese eee eneceeeees 5 24 PRUNE esd a aE E aa 5 24 s riak Looten eas 5 24 connection autosampler CUSTOMET SELVICE ssissseeeeeeeereeere ereere 10 3 cyanide solutions Safety iaaa aa 2 7 D deuterium arc background corrector ACCESSOTIES eig t ei aes 9 53 Cescription s s5 te eesieceieec ies 4 11 TeasseMbIing eee eeeeeseeneeeneees 9 48 removing lamp assembly 9 46 replacing lamp ce ceeeeeseeeeeneees 9 46 replacing lamp ces eeeeeeseeseeeneees 9 47 troubleshooting 10 13 display CONECO oee nee EEEE 5 24 drain system ACCES SOFIES ertoe Er eia E 9 53 cleaning the system cece 9 30 CeSCHIPtION rissin ieiit inss 4 16 drain float adding water 9 30 9 31 flushing the system sseeeeeeeseeee 9 30 maintenance eeeeeseeeeeereereerereee 9 29 maintenance checklist eee 9 9 TUBING oi ethene aati nein ss 9 30 tubing prepare new for use 9 31 t
58. 2 7 Chemicals s suisse acetates 2 20 3 6 Compressed gases 2 14 correct use of the instrument 2 4 cyanide solutions s es 2 7 electrical safety 0 0 cee cee eeeeeeeeeeees 2 13 gas cylinders 0 eee ionin 2 15 gases DUET inspicit aaas 2 17 high temperatures 0 00 cccceeseeeeeeees 2 12 references for lab safety practice 2 23 use of burner gases seee 3 16 UV radiation oseere 2 11 safety checks D mer anomenen iee rt s 6 26 safety conventions see also symbols symbols used in the guide 2 8 Safety information sesser 2 5 safety practices flame atomization cece eee 2 10 sample shelf Installation ele eee cese cess eeteeeeeeeees 5 22 Serial 1 CONNECTION eee eeteeeteeeeeees 5 24 servicing aUtosaMplel cee eeeceeeeeeeeeeeeeeeeeeee 9 50 setting UP EMISSION ee eeeeeeseeeeeneees 8 23 shipment inspection eee eee ceteeees 5 4 l 7 Index Shipping list eioten raise anst 5 8 Sh tdO WN ieres ie ae ia e ea 8 31 slot width burner h adan 9 19 spacer Installing senen o a 9 35 spare PaltSscerc duress vosit Seteasecoeevieesdevestees 5 9 autosampler 0 eee eee eseceeeceteeeeeees 9 50 OPderNg ogies Meee eet 9 54 specifications acetylene isei nin i 3 18 electrical supply ssssesssesesseessseeseees 4 19 spectrometer ACCESSOTI ESen e iE aie 9 54 SWATCH E T 6 25 unpacking soeren ewe teste 5 4 standard concentrations entries on calibra
59. 37 1492 and locking ring 8 Remove the capillary assembly from the nebulizer body Cleaning While holding the capillary assembly in one hand take one of the cleaning wires P N 0303 1 0135 supplied 2 Push it through the capillary assembly from its wider open end NOTE It may take several attempts to pass the wire through the nebulizer 9 38 AAnalyst 200 User s Guide A Alignment l Keyway Impact Bead A Structure Nebulizer Spacer O Rings End View N OP Locking Ring Adjusting Nut sy ae Nebulizer Side ey Capillary Screw R is O O Ring M Capillary Holder Alignment Key Gas Supply Connector Nut Figure 9 13 Standard nebulizer assembly Removing and replacing the nebulizer s impact bead The AAnalyst nebulizer utilizes a ceramic one piece impact bead structure P N B050 5086 which improves nebulization efficiency The bead itself is held by two fragile support arms The bead structure mounts directly on the nebulizer s body assembly see Figure 9 14 To Install Impact Bead 1 Hold the impact bead by its base and carefully push it onto the body of the nebulizer in front of the venturi Then rotate it holding only the base approximately 1 8 turn clockwise i e until it reaches a stop 9 39 Maintenance To Remove Impact Bead 1 Hold the impact bead by its base only 2 Rotate it approximately 1 8 turn counter clockwise before carefully li
60. 4 A successful download will display Download is Completed on the command prompt 5 Reboot the AAnalyst 200 instrument by powering it down and back up 7 44 AAnalyst 200 User s Guide A WINNT System32 cmd exe A z gt CeRun storage card killer exe A gt CeCopy pe IP_storage2reg exe ce storage card IP_storage2reg exe Copying PC IP_storage2reg exe to CE IP_storage2reg exe 2566 bytes in 3 sec A gt CeCopy pc autosamp htm ce storage card web autosamp htm Copying PC autosamp htm to CE autosamp htm 9438 bytes in 4 sec A gt CeCopy pe flame db ce storage card db f lame db Copying PC flame db to CE flame db 15320 bytes in 8 sec Az gt echo Download is completed Download is completed A gt pause Press any key to continue Screen 7 33 Command Prompt Window Application Launch Failure Use the following procedure below if the application fail to launch 1 2 3 Follow steps 1 4 from the Connection Setup procedure Connect the keyboard to the E Box Power on the AA200 instrument and wait until the screen shows an arrow on top of the splash screen Timing is crucial just as the arrow appears use the keyboard to press the ESC key continuously until a blue PerkinElmer Instrument screen appears on the touch screen NOTE Press CTRL ESC key to display the Start menu 5 6 Use the arrow keys on the keyboard to Select Run or touch Run on the touch scre
61. 9 9 is recommended A high quality filter dryer accessory is recommended for the removal of any moisture from the purge gas 4 Turn the gases on Test all gas connections for leaks using an approved gas leak detection fluid 5 14 AAnalyst 200 User s Guide eal NO Air CH ear Blue Black Red Figure 5 5Rear view of the spectrometer showing the gas hoses Connecting to the air supply Warning Flashback Hazard PerkinElmer burner systems are designed for use with compressed air The use of oxygen can cause an explosion in the burner system and oxygen enriched air can cause a flashback of the flame Never use oxygen or oxygen rich air with PerkinElmer burner systems Use only compressed air WARNING 5 15 Installation Compression nut Air Supply Black air hose from spectrometer Air dryer filter assembly Figure 5 6 Air supply connections showing air dryer filter assembly 1 Connect the black air hose coming from the back of the spectrometer to the outlet of the air dryer filter assembly 2 Tighten the connection using the double wrench technique Hold the fitting on the air dryer filter assembly with one wrench and tighten the compression nut on the gas hose with the other wrench Screen 5 6 Double Wrench technique 5 16 AAnalyst 200 User s Guide Connecting to the nitrous oxide supply i Nitrous oxide regulator Compression nut f Nitrous oxide cy
62. AAnalyst 200 User s Guide Release History Part Number Publication Date 0993 6594 April 2006 Any comments about the documentation for this product should be addressed to User Assistance PerkinElmer Inc 710 Bridgeport Avenue Shelton Connecticut 06484 4794 U S A Or emailed to info perkinelmer com Notices The information contained in this document is subject to change without notice Except as specifically set forth in its terms and conditions of sale PerkinElmer makes no warranty of any kind with regard to this document including but not limited to the implied warranties of merchantability and fitness for a particular purpose PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with furnishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may be reproduced in any form whatsoever or translated into any language without the prior written permission of PerkinElmer Inc Copyright 2006 PerkinElmer Inc Trademarks Registered names trademarks etc used in this document even when not specifically marked as such are protected by law PerkinElmer is a registered trademark of PerkinElmer Inc AAnalysts and e ssentials are trademarks of PerkinElmer Inc Table of Contents Chapter 1 Introduction Abo
63. Depending on your system you may have a single lamp or multi lamp configuration For procedures on how to install and align lamp see Chapter 6 Operation of the Instrument Make sure the lamps are properly installed and aligned then follow the steps below for entering analytical parameters On the lamp page the lamp element s are displayed on the upper portion of the screen e For a coded lamp no entries are required for the lamp parameters The parameters are automatically supplied and filled according to the recommended conditions by the system Touch Screens e For an uncoded lamp you must complete the following entries Element Lamp Type and current The Wavelength and Slit Width are automatically filled in after entering the element symbol Coded Lamp Single Element Coded Lamp 1 3 If you installed a single element coded lamp the analyte appears automatically in the element entry field box To change entries of other recommended parameters Wavelength Slit Signal touch the entry field box to display dialogs Touch the Install Lamp button to make changes to the recommended parameters in the Install Lamp dialog When lamp parameters are properly set up touch the Setup Instrument button Multi Element Coded Lamp 1 Ifyou installed a multi element coded lamp touch the Elements entry field box to display the Element dialog Select the required analyte element from the list in the dialog and the recommended par
64. E Box Align the lamp NOTE Example If the EDL lamp is installed in position 1 of the turret connect the EDL cable to the EDL 1 port on the E Box 6 23 Operation of the Instrument Removing lamps 1 2 6 ts Do not unplug and remove lamps while they are switched on Touch the Lamp tab to display the Lamp page On the Lamp page touch the Install Lamps button The Install Lamps dialog is displayed Make sure that the lamp is switched off before you remove it The On Off box must not be checked If necessary touch the respective On Off box to switch off the lamp Touch OK Unplug and remove the lamp For EDLs remove the coding plug as well Tips for installing lamps e Use PerkinElmer lamps e Do not touch the front window of the lamp perspiration or other contamination can reduce intensity of the radiation e With EDLs make sure that you use the correct coding plug and connect it to the receptacle on the lamp holder containing the EDL e If you use the wrong coding plug you will cause the spectrometer to malfunction and may cause irreparable damage to the lamp 6 24 AAnalyst 200 User s Guide Switching on the Spectrometer a aia hr liege Fr AN N P aN SEA aie oe Ae On Off Switch Figure 6 13 Location of operational on off switch 1 Open the lamp door 2 Switch on the spectrometer with the operational on off switch 3 Close the lamp door 4 Wait for the spectrom
65. Fuel and oxidant gas lines may have been inadvertently switched The burner system may leak AAnalyst 200 User s Guide Try igniting the flame a second or third time Carefully inspect the burner system for possible causes referring to the ones listed below Reignite the flame only after the problem has been corrected Contact a PerkinElmer service representative for assistance Check the connections at the burner and at the gas supplies Check the condition of all o rings burner head end cap o ring on nebulizer front end cap Replace o rings that show signs of wear cracking swelling Inspect the inner surface of the burner chamber for pitting and replace if necessary Check drain connections for leaks 10 9 Troubleshooting Burner flashes back continued 10 10 Possible Cause of Problem There may be a break or leak in the drain tubing The burner head may be clogged Gas flows may be set incorrectly Gas connections may be loose or a leak may have occurred The air supply may contain excess oxygen The wrong gas supplies may be in use Check and or Remedy Inspect tubing and replace if necessary Check the burner head and clean if necessary If running samples in organic solvents a flame that is too lean can cause a flashback If a lean flame is required adjust the nebulizer uptake rate If you suspect a leak in the gas lines immediately close the cylinder valve If you ne
66. NG This symbol alerts you to the risk of electric shock that could result in personal injury to yourself or other persons Details about these circumstances are in a box like this one WARNING This symbol alerts you to the risk of hot surfaces that could cause personal injury to yourself or other persons Details about these circumstances are in a box like this one WARNING We use the term CAUTION to inform you about situations that could result in serious damage to the instrument or other equipment Details about CAUTION these circumstances are in a box like this one 2 8 AAnalyst 200 User s Guide Symbols Used on the Instrument Any of the following symbols can be used on the instrument Caution risk of electric shock Caution hot surfaces Caution risk of danger Documentation must be consulted to determine the nature o the potential hazard and any actions which have to be taken Indicates alternating current Indicates the off position of the main power switch Indicates the on position of the main power switch Indicates the protective conductor terminal 0O ep P Safety Practices Safety Practices for Flame Atomization Safe operation of the flame Before you ignite the flame make sure that The laboratory exhaust venting system is operating The burner head is installed correctly The burner end cap is secured firmly The burner unit contains the necessary solvent resistant components if
67. OTE Preparing Your Lab When you remove the instrument from storage and before you put it into operation allow it to stand for at least a day under the recommended operating conditions Laboratory hygiene Keep the work area scrupulously clean to avoid contaminating your samples and to maintain a safe working environment Clean up spilled chemicals immediately and dispose of them properly Do not allow waste to accumulate in the work area Dispose of waste correctly Do not allow smoking in the work area Smoking is a source of significant contamination and also a potential route for ingesting harmful chemicals Do not store handle or consume food in the work area Working with chemicals Some chemicals used with the instrument may be hazardous or may become hazardous after completion of an analysis Use store and dispose of chemicals in accordance with the manufacturer s recommendations and the applicable national state and or local regulations Do not put open containers of solvent near the instrument Store solvents in an approved cabinet with the appropriate ventilation away from the instrument Wear appropriate eye protection at all times while handling chemicals Depending on the types of chemicals you are handling wear safety glasses with side shields or goggles or a full face shield Wear suitable protective clothing including gloves if necessary resistant to the chemicals you are handling When pre
68. Tighten the four clamp adjusting screws Replacing or Installing the MHS 15 Quartz Cell onto the Holder After installing the cell holder install the quartz cell as follows 1 Rotate the cell holder bracket to the up position 2 Place the quartz cell in the cell holder as shown in the next figure Be certain that the transfer hose cannot become pinched or kinked in any way A restriction in the hose may lead to a pressure build up in the system which can cause an explosion WARNING 9 58 AAnalyst 200 User s Guide Figure 9 23 Installing the quartz cell onto the holder 3 Carefully lower the cell holder bracket to the down position 9 59 Maintenance Replacement Parts and Accessories The following is a partial list of common consumable parts and accessories For more information refer to the e ssentials catalog Burner Head and Accessories Description PE Part Number 5 cm single slot N 0 Acetylene N040 0100 5 cm single slot air Acetylene N040 0101 10 cm single slot air Acetylene standard N040 0102 10 cm three slot air Acetylene N040 0103 Flow spoiler 0057 2561 Burner Head cleaning tool 0303 1573 AAnalyst 200 400 Nebulizer kit N315 0188 Burner Gasket Kit Description PE Part Number O Ring Standard 0990 2147 Burner Cap Organics Corkprene 0047 2014 Organics Kalrez 0992 1044 O ring for the burner head 0990 2219 Ne
69. To analyze the standard indicated in the standard concentration box touch this button A green light appears on the button when selected The system analyzes the standard and creates a calibration curve Standards can be reanalyzed by selecting the standard from the Standard Concentration Box To analyze the sample indicated by the sample number entry field touch this button A green light appears on the button when selected Samples can be reanalyzed by selecting the sample from the Sample Number Box To display the calibration curve window touch this button By default the print function is On and the results will print when the printer queue is full The green light indicates that it is On To turn print function Off touch Printer On Off button You may print the results without waiting for the printer queue to fill up by touching the Printer On Off button Items on Analyze Samples page Standard Concentration Box Touch this entry field box to view the standard concentration dialog Use the dialog to select the standard concentration you want to analyze A calibration curve is created after blank and selected standard are run Sample Number Box This entry field shows the sample No of the sample you are ID Number Box Dilution Box 7 22 currently analyzing If you wish to analyze a different sample touch this entry field box to view the sample number dialog This entry field allows you to enter the ID number for th
70. Units On Parameters page Calibration subpage Standard Concentrations section 1 Enter the concentration of the first standard for the element that you are determining e g 0 5 mg L for copper 2 Enter the concentration of Standard 2 for the element you are determining e g 1 0 mg L for copper 3 Enter the concentration of Standard 3 for the element you are determining e g 1 5 mg L for copper For the above example we will only be calibrating with three standards e Fnter the concentration of the Reslope standard e g 5 mg L for copper 8 18 AAnalyst 200 User s Guide Calibration fect Calibration Equation Linear Through Zero P 4 Calibration Units Jenga Standard Concentrations Figures After Decimal B ihso o aoo 2 s000 fl 310 000 oo a Reslope 5 000 HN FE Parameters j Screen 8 10 Parameters page Calibration subpage Parameter entry is now complete on the Parameter page At this point the autosampler tray should be filled with blank standards and samples All of the parameter entries on the Analyze page should be completed by now Proceed to the next step Analyze Page The results appear on the analyze screen in the order of the solutions analyzed The most recent results are displayed at the top of the screen e Touch the Analyze tab to display the Analyze page e Touch the Printer On Off button if you wish the results to be printed Calibrate Use this procedure
71. User s Guide References for Laboratory Safety Practice 1 Bretherik L Bretherik s Handbook of Reactive Chemical Hazards 4th ed Butterworth amp Co Ltd London UK 1990 2 Safe Practices in Chemical Laboratories Royal Society of Chemistry London UK 1989 3 Hazards in the Chemical Laboratory 5th edition Luxon S G ed Royal Society of Chemistry London UK 1992 4 CRC Handbook of Laboratory Safety 4th edition Furr K ed The Chemical Rubber Co Press Florida USA 1995 5 Prudent Practices for Handling Hazardous Chemicals in Laboratories National Research Council National Academic Press Washington D C USA 1981 6 Sax s Dangerous Properties of Industrial Materials 9th edition Sax N I and Lewis R J eds Wiley New York USA 1998 7 Pohanish R P and Greene S A Hazardous Materials Handbook Wiley New York USA 1996 8 Compressed Gas Association Inc Arlington VA 22202 USA various publications 9 Data Sheets provided by chemical manufacturers e g USA Material Safety Data Sheets MSDS FRG DIN Sicherheitsblatter UK Hazard Data Sheets 2 25 Safety Practices 2 26 Preparing Your Lab AAnalyst 200 User s Guide Introduction The AAnalyst 200 spectrometer has some special requirements that you must consider when setting up the laboratory The items shown in the following checklist need to be considered when preparing the laboratory for the instrument
72. YNC EXE file A dialog will appear indicating that MS Active Sync is being extracted 5 Following extraction of MS Active Sync a Setup dialog will appear Microsoft ActiveSync Set Up Microsoft ActiveSync 3 5 Before you can exchange information between your mobile device and this computer you must set up ActiveSync This setup wizard will guide you through Installing the ActiveSync program on this computer Setting up your mobile device Note It is strongly recommended that you exit all Windows programs before continuing with this setup wizard Click Next to continue with the setup process Click Cancel to quit setup Cancel Help Screen 7 35 Microsoft ActiveSync Install Shield 6 Proceed with the setup by clicking Next on each page that appears 7 Connect the serial cable part number 0941 0063 to the serial connections on the front of the AAnalyst 200 E Box and at the rear of the computer 7 47 Touch Screens 8 Power on the AAnalyst 200 if it is not already on 9 On the AAnalyst 200 touch screen touch the Tools button to access the Tools dialog 10 From the Tools dialog touch the Download button Screen 7 36 Tools Dialog from the Touch Screen 11 A message indicating System will stop the application to prepare for a download will appear Touch OK 12 If a partnership dialog box appears on the computer screen select the No option button and then click Next NOTE
73. ab 9 Select the Parameters page Calibration tab In the Calibration Equation field touch the screen to access the dialog 8 28 AAnalyst 200 User s Guide Linear Through Zero Ay a a x x a a x A x a x a ax a x A ax a x Screen 8 19 Parameters page Calibration tab 10 In the Calibration Equation dialog touch the appropriate calibration equation radio button to change the calibration equation Touch the OK button to close this dialog box NOTE In the Calibration Equation window Linear Through Zero is the default choice for Flame Emission 8 29 Analyzing Samples Calibration Calibration Equation Linear Through Zero 4 A Calibration Equation Calibration pesto Nonlinear Through Zero Cancel Linear Through Zero Method of Additions Sample Intercept Method of Additions Calibrate Linear Calculated Intercept Method of Additions Calculated Intercept Linear Bracketing E i i Cok Cece cece A SA cece cece oe oh CR ce oe oe oe am g C a a Cc Co CT Cc n Parameters Tools Screen 8 20 Parameters page Calibration tab 11 Go to the Analyze Sample page to start the analysis Touch the Analyze Blank Standard or Sample bar to begin the analysis If printed results are needed touch the Printer On Off bar to print the results Analyze Blank Auto Scale Graph Analyze Standard Standard 1 0 500 mg L Display Calibration
74. ace The ignitor arm is a gas capture tube through which the gases flow from the burner to the glow plug The gases in the tube are ignited by the heat of the glow plug which in turn ignite the flame at the burner head slot The gas controls The gas controls provide control of the flow rates of the fuel gas acetylene and the oxidant air or nitrous oxide You select the gas flow rates and optimize the flame via the touch screen The gas control system is incorporated in the spectrometer The system includes safety interlocks for the flame If the fuel or oxidant pressure falls below a minimum value the flame is shut down in a safe sequence The system also includes automatic sequencing of the gases when the nitrous oxide acetylene flame is ignited or extinguished The burner will be shut down in a safe sequence in the event of a power failure In case of emergency use the red emergency button located on the upper left hand side of the instrument The drain system During flame operation measurement solution that condenses out in the spray chamber runs to waste through the siphon interlock drain trap and is collected in the drain vessel The siphon interlock drain trap is integral with the burner end cap and includes an internal trap to make certain that back pressure is applied to the burner chamber This ensures that a fuel oxidant mixture cannot enter the drain vessel There is a magnetic float in the drain trap that shuts down the
75. aces of the solvents from the system e Ifthe sample solutions contained toxic substances you must rinse all traces of these substances out of the system e Ifthe sample solutions contained high concentrations of copper silver or mercury salts which can form unstable acetylides you must rinse all traces of these substances out of the system Procedures If you used only aqueous solutions during the analyses e Aspirate deionized water for 5 minutes If you used organic solvents during the analyses e Aspirate for 5 minutes an organic solvent that is miscible with the samples that have just been aspirated e Aspirate for 5 minutes methanol or another solvent that is miscible both with water and the solvent used previously e Aspirate 1 v v nitric acid solution for 5 minutes e Aspirate deionized water for 5 minutes 8 33 Analyzing Samples 8 34 Maintenance Q AAnalyst 200 User s Guide Introduction This chapter describes the routine maintenance procedures required to keep your instrument in proper working condition and to ensure the highest possible level of performance It includes maintenance checks that should be done on a daily basis and maintenance procedures that should be done periodically depending on instrument use This chapter is divided into several sections each section covering maintenance procedures for a particular component of the system You should perform only the maintenance procedures descr
76. ake the instrument inoperative and secure it against any unauthorized or unintentional operation The electrical safety of the instrument is likely to be impaired if for exam ple the instrument shows visible damage has been subjected to prolonged storage under unfavorable conditions or has been subjected to severe stress during transportation 2 13 Safety Practices Compressed Gases NOTE The permanent installation of gas supplies is the responsibility of the user and should conform to local safety and building regulations Warning Compressed Gases High pressure gas cylinders can be dangerous if mishandled or misused You WARNING must have a tank regulator on the gas cylinder NOTE The responsible body must ensure that the type of connector used at the outlet side of the gas pressure regulator conforms to applicable national requirements Summary of gas hazards Hazards associated with the different gases used in atomic absorption spectrometry are presented in the table below or Combustion Air ee S y Argon o a o e y Nitrogen CT o a o e o y Acetylene ethyne C2H8 x x x y y Nitrous Oxide dinitrogen x monoxide N20 Contact the gas supplier for a material safety data sheet MSDS containing detailed information on the potential hazards associated with the gas Warning Nitrous oxide is a strong oxidant and an asphyxiant Nitrous oxide is an asphyxiant it can be considered a potential hazard wheneve
77. al and electrical components and is aware of the hazards of high voltage electronics WARNING Equipment Needed You ll need to gather the following items in order to replace the deuterium lamp e the deuterium arc lamp P N B315 0160 e ultraviolet absorbing safety glasses e flat bladed screwdriver e phillips head screwdriver Removing the Deuterium Lamp Assembly 1 Turn OFF the power switch and unplug the power cord from the E Box Wait a sufficient amount of time for the background corrector lamp to cool before replacing it WARNING The lamp is very hot after use 2 Swing open the lamp compartment door 3 Locate the deuterium lamp assembly in the instrument it is inside the large rectangular block to the right of the lamp compartment 4 Unscrew the 4 corner phillips screws that hold the deuterium lamp plate in place Don t let any of the 4 screws drop into the instrument 5 Carefully lift the assembly away from the housing and unplug the deuterium connector 6 Remove the assembly completely from the instrument and place it on the lab bench 9 52 AAnalyst 200 User s Guide Figure 9 18 Deuterium lamp assembly Replacing the Deuterium Lamp Use great care when handling the deuterium lamp it is fragile When handling the new lamp do not handle the glass only the metal lamp bracket You don t want to get fingerprints on the viewing area of the lamp as CAUTION this will decrease the UV perfo
78. als as large as 3 absorbance units The background corrector is internally installed with its power supplied from the instrument Power to the source is automatically and continuously adjusted to be in the optimum range for operation The deuterium arc lamp is easily accessible allowing convenient replacement of the lamp by the users Instructions to replace the lamp are included in the Maintenance chapter Deuterium Alignment Refer to Chapter 6 Operation of the Instrument in this manual for the procedures to align the background corrector in an AAnalyst instrument System Description The Burner System The burner system used in the spectrometer system is of the premix design The measurement solution is sprayed by a pneumatic nebulizer into the burner chamber in the form of an aerosol This aerosol is thoroughly premixed with the burner fuel and oxidant gases in the burner chamber This gas mixture then passes through the burner slot into the flame The burner system comprises the following major components e Nebulizer e Burner chamber including the flow spoiler and end cap e Burner head e Drain system e Gas control system incorporated in the spectrometer Burner Head Burner Mixin Flow Spoiler ene Impact Bead Structure Spacer O Rings Nebulizer Body E Nebulizer Side Arm Drain Figure 4 7 Major components of the burner system 4 12 AAnalyst 200 User s Guide How the Burner Syste
79. amber apart 8 Remove the standard o ring from the end cap and carefully fit the solvent resistant o ring 9 Reassemble the burner system 6 11 Operation of the Instrument Installing the Burner Mount Assembly OSO Figure 6 6 Installing the burner mount assembly 6 12 AAnalyst 200 User s Guide Orient the assembly to slide into the tracks as shown in the figure above Slide the assembly along the tracks into place in front of the instrument When the assembly is pushed all the way in you will hear a clicking sound as the three fittings seat themselves and lock into the back of the sample compartment Pull the lever forward to lock the burner mount Warning Flashback While the flame is on DO NOT push the lever that is located on the burner mount assembly WARNING 6 13 Operation of the Instrument Installing the Burner Drain System Locate and unpack the drain system from the shipping carton It includes all the parts marked in the figure below Connecting the Burner Drain System 1 Refer to the next figure when installing the drain system Position the vessel on the floor underneath the front of the instrument and attach the retainer cap assembly cap trap and loop to the drain vessel 2 Hold up the free end of t
80. ameters for that element are set up 2 To change entries of other recommended parameters Wavelength Slit Width Signal touch the entry field box to display dialogs Touch the Install Lamp button to make changes to the recommended parameters in the Install Lamp dialog 3 When lamp parameters are properly set up touch the Setup Instrument button Uncoded Lamp If you installed a single element or multi element uncoded lamp follow the steps below l 7 10 From the Lamp page touch the Install Lamp button The Install Lamp dialog appears and you must manually input the required entries for each of the parameters To input entries touch on the entry field box and a dialog or keypad will display After all entries are made for each of the parameters touch OK to return to the Lamp page On the Lamp page touch the Elements entry field box to select an element When lamp parameters are properly set up touch Setup Instrument button AAnalyst 200 User s Guide Flame page You use this page to select the oxidant and other flame parameters and to ignite the flame You also use this page during optimization of the burner system and to view continuous graphical absorbance display Bleed Gases Oxidant Air Auto Scale Graph f Auto Zero Graph Oxidant Flow L min l jo 20 p _Autozeroorann Acetylene Flow L min a 3 70 gt Screen 7 6 Flame Page To switch oxidant type 1 Shut off the flame and wait until the burner
81. an the surfaces as described above Special care must be taken to avoid scratches which would require replacement of the mirrors 9 5 Maintenance Never touch or clean the grating surfaces Fingerprints or scratches will adversely affect the dispersion characteristics of the grating and CAUTION impair the operation of the instrument Cleaning the Instrument Exterior surfaces may be cleaned with a soft cloth dampened with a mild detergent and water solution Do not use abrasive cleaners or solvents Use the same technique to clean the sample compartment windows too AAnalyst 200 User s Guide Checks Periodic Checks The frequency of maintenance required will be determined by the amount of use the system receives the cleanliness of the environment and the number and nature of the samples being analysed Instrument parts that require periodic checks e Nebulizer Check the wear and tear of the o rings on the end caps and on the burner head To replace the o rings see Disassembling the Burner Chamber later in this chapter e Drain System Maintenance Check for wear and or chemical attack The drain tubing should be clear with as few bends as possible The drain system should be replaced if it has deteriorated See Drain System Maintenance later in this chapter e Burner System Check for uneven flame and deposits build up along the burner slot e Air Filters Should be replaced yearly or as needed in a dusty enviro
82. and the solvent used previously e Aspirate 1 v v nitric acid solution for 5 minutes e Aspirate deionized water for 5 minutes To extinguish the flame 1 With the flame still burning aspirate the correct rinsing solutions to rinse the burner system Either aspirate the solutions manually or use the flame autosampler 2 Touch the Flame tab to display the Flame page 3 Touch the Off side of the Flame On Off switch The indicator in the switch extinguishes The system uses a predetermined shutdown sequence to extinguish the flame safely 4 Shut down the gases to the spectrometer at source 5 Touch the Bleed Gases button to depressurize the gas lines 6 43 Operation of the Instrument 6 44 Touch Screens AAnalyst 200 User s Guide User Interface Signal Atomic Absorption Set Midscale Cu Element Setup Instrument Wavelength nm 324 75 Slit mm 2 7 0 8 Install Lamps Screen 7 1 Typical Touch Screen Display Touch screen You operate the spectrometer using the touch screen The touch screen is the interface between you and the spectrometer enabling you to control the spectrometer in order to perform your analyses easily and conveniently The touch screen contains active areas that you touch to perform the required action Only use the stylus provide with your AAnalyst 200 to touch the active areas of the touch screen Do not use sharp pointed objects A light short touch is all that is need
83. and then use this calibration curve to measure all subsequent samples This option allows the intercept of the calibration curve with the absorbance axis to be calculated rather than forced through zero In the calculation algorithm the blank solution is treated as another point on the curve You select the analyte addition technique when the composition of the unknown sample is unknown and the matrix causes an interference that varies in magnitude from sample to sample With this technique every unknown sample is calibrated individually The intercept of the calibration curve with the absorbance axis is calculated rather than forced through zero This option is applicable over a restricted concentration range at higher concentration levels The concentrations of the standards bracket the concentrations of the unknown samples and only a limited section of the calibration curve is used for the evaluation 7 19 Touch Screens Analyze Page Manual Data Display This window allows users to manually analyze a solution and view the results in the Result Window that appears on the Analyze Sample Page When the system finishes the analysis of each solution data will appear at the bottom of the scrolling display as it is generated and the user will have the option of scrolling backward to review previous data If a sample information file is being used the sample location must be re entered on this screen to populate the Sample ID and Dilutio
84. anel of the AAnalyst 200 oooooooo0oo0o000000000000000000000000000000000000 oooooo00000000000000000000 oooo000000000 oOoo0o00000000000000000000000 oo0o00000000000 ooooooooo00000000000000000 ooooo0o00000000 ooooo0o000000000000000000000000000000000000000 oooooooo0o0000000000000000000000000000000000000 AAnalyst E Box P PerkinElmer instruments Shelton CT 06484 USA AAnalyst E Box PartNo Serial No Made in Singapore WARNING To prevent a shock hazard turn the power switch off and unplug the AC line cord from the AC outlet WARNING To reduce the chance of an electrical shock do not remove covers that require tool access No user serviceable parts are inside Refer servicing to PerkinElmer qualified service personnel 1 11 Introduction Safety Practices AAnalyst 200 User s Guide Chapter Overview This chapter describes the general safety practices and precautions that must be observed when operating the AAnalyst 200 This advice is intended to supplement not supersede the normal safety codes in the user s country It is also a supplement to the PerkinElmer standard Safety and Health Policy The information provided does not cover every safety procedure that should be practiced Ultimately maintenance of a safe laboratory environment is the responsibility of the analyst and the analyst s organization Please consult all manuals suppl
85. ard button e Aspirate Standard 3 then touch the Analyze Standard button 8 8 NOTE NOTE AAnalyst 200 User s Guide After a standard is analyzed the next standard concentration is automatically incremented in the standard entry field box You have the option of using the automatically filled entry or you may select a different standard concentration to be analyzed by using the standard touch entry field box The dialog displays a list of standard concentrations that you can choose from Run the samples e Aspirate Sample 1 and then press the Analyze Sample button e Aspirate Sample 2 and then press the Analyze Sample button After a sample is analyzed the next sample ID is automatically incremented in the sample entry field box You may enter a sample number by touching the sample entry field box to use the keypad Run the reslope standard 1 Analyze the blank 2 Aspirate the Reslope Standard we used Standard 2 for our Reslope Standard then press the Analyze Standard button Run the remaining samples 1 Aspirate Sample 3 and then press the Analyze Sample button 2 Aspirate Sample 4 and then press the Analyze Sample button The results are displayed and printed Standard 1 0 0006 0 6 Standard 2 0 0007 0 4 Standard 3 0 0009 0 3 Analyze Blank Printer On Off Analyze Standard re Standard 1 0 500 mg L Display Calibration Analyze Sample A ID Sample 001 Dilution 1 000 Parameters i Tools Sc
86. as an absorbing wavelength above 250 nm and whose sensitivity is not dependent on the fuel oxidant ratio Do not select an element requiring a nitrous oxide acetylene flame If necessary adjust the burner height using the procedure described in Chapter 6 Operation of the Instrument Aspirate a blank and let the flame stabilize as described Chapter 6 Operation of the Instrument If you see bubbles at the end of the capillary tube in the sample solution loosen the nebulizer locking nut and slowly turn the adjustment nut clockwise until the bubbling stops Aspirate a standard and adjust the burner position as described in Chapter 6 Operation of the Instrument Optimize the burner position by using the rotational and horizontal adjustment knobs identified in Chapter 6 Operation of the Instrument While still aspirating the standard turn the nebulizer locking nut clockwise until it is free of the nebulizer adjustment nut Slowly turn the nebulizer adjustment nut counter clockwise until bubbles begin to appear at the end of the capillary tube in the sample solution Slowly turn the nebulizer adjustment nut clockwise until the absorbance goes to a maximum and then begins to decrease Lock the nebulizer adjustment nut in its current optimum position by turning the nebulizer locking nut counter clockwise while carefully holding the nebulizer adjustment nut Check the characteristic concentration as instructed in the User s Guide Us
87. as cleaning You must always preadjust the nebulizer before you optimize the nebulizer see chapter 9 Maintenance Warning Flashback Hazard Never preadjust the nebulizer using a nitrous oxide acetylene flame WARNING Preadjust the nebulizer using an air acetylene flame only and make small adjustments slowly Preliminary steps Prepare a blank solution and a standard solution of an element that requires an oxidizing blue air acetylene flame and whose analytical line lies above 250 nm Recommended elements Cu 324 8 nm Mg 285 2 nm or Pb 283 3 nm Do not use an element that is sensitive to the air fuel ratio of the flame e g Ca Cr Pd Pt Rh Ru Au and Ir The concentration of the standard solution should be in the linear range and ideally should be close to the sensitivity check concentration quoted in the Recommended Conditions i e give an absorbance reading of approximately A 0 2 You use this element to preadjust the nebulizer It may be different to the element you subsequently analyze 1 Install a lamp for the element you have chosen 2 Start up the spectrometer 3 Set up the burner system 4 Perform the safety checks Ignite the flame 5 Touch the Lamp tab to display the Lamp page 6 For Signal select AA no corrected or AA background corrected if you will be using background correction later 6 37 Operation of the Instrument Preadjustment procedure 1 2 Touch the Fla
88. at these sources be of similar intensity and pass through exactly the same area of the sample cell There are three possible problems that may be observed when the background corrector source lamp is not aligned or needs replacing e Measurements are excessively noisy e The intensity of the background source may be much less than the intensity of the primary source e Background absorbance may not be properly corrected You can check this by measuring a sample containing only matrix components with no analyte These problems indicate that the background corrector source is either not properly aligned or should be replaced Refer to the section called Replacing the Deuterium Lamp in Maintenance chapter if it needs replacing Possible Cause of Problem Background source May not need to use the intensity is much background corrector lower than the primary source The intensity is not matched The deuterium lamp may need replacing B315 0160 Check and or Remedy Determine if the background corrector should be used It is useful up to about 400 nm 1 Reduce the hollow cathode or the EDL current in order to reduce the primary source intensity This may increase the noise for the determination 2 In addition or alternatively increase the slit width this may increase the possibility of spectral interferences or increase the calibration curvature Replace the lamp 10 13 Troubleshooting 10 14 Index
89. ater If they look damaged replace them After you have cleaned the components reassemble the nebulizer 9 43 Maintenance Reassembly and Replacement Reassembling the nebulizer NOTE f not already done inspect the tiny o rings on the capillary assembly for damage and replace them if necessary Lightly lubricate the surface of the o rings with a minimum of Apiezon grease Make sure that no grease gets onto the tip of the capillary Do not add an excess of Apiezon grease Lightly lubricate the surface of the o rings Too much grease on the o rings will affect instrument performance CAUTION 1 Slide the spring back onto the capillary assembly if it was removed 2 Slide the assembled capillary assembly into the nebulizer body 3 Line up the alignment key with the keyway in the nebulizer body 4 Push the capillary assembly in until it bottoms out in the nebulizer body 5 If you inserted the capillary assembly correctly it should move freely in and out of the nebulizer body If it does not remove and reinstall paying particular attention to the alignment key 6 Screw the adjusting nut onto the nebulizer body 7 Where applicable refit the fragile impact bead and spacer 8 Reattach the nebulizer sample tube to the nebulizer by screwing the connector into the nebulizer body 9 Reinstall the nebulizer in the end cap 9 44 AAnalyst 200 User s Guide Replacing Parts of Wear Burner System O Rings The
90. ation of the analyte in your Zero Linear Through Zero Through Zero Method Addition 7 18 samples to be outside the linear range This option covers the widest concentration range and you need a larger number of standards calibration solutions to establish the calibration curve A calibration curve defined using this equation is forced to pass through zero absorbance and zero concentration i e the origin Select this option if you expect the concentration of the analyte in your samples to be within the linear range A calibration curve defined using this equation is forced to pass through zero absorbance and zero concentration i e the origin You select the analyte addition technique when the composition of the sample is unknown and the matrix causes an interference that varies in magnitude from sample to sample With this technique every unknown Analyte Addition Calibrate Calculated Intercept Linear Calculated Intercept Analyte Addition Bracketing Calibration AAnalyst 200 User s Guide sample is calibrated individually A calibration curve defined using this equation is forced to pass through zero absorbance and zero concentration i e the origin You can select the technique of addition calibration when the matrix causes interference but the matrix is consistent in all the unknown samples You establish the calibration curve for the first unknown sample using the analyte addition technique
91. atomization e Deuterium background correction system optional System components The major components of the system are e The spectrometer containing the optical system the electronics and the atomizer compartment e The touch screen is the interface between you and the spectrometer enabling you to control the spectrometer in order to perform your analyses easily and conveniently e The burner system e The printer This is optional but strongly recommended System control To control the spectrometer and perform your analyses you use the touch screen When you switch on the spectrometer system it performs an initialization procedure to check the instrument While the spectrometer is operating the control system continually monitors many instrument functions It generates appropriate messages when a problem occurs and prevents potentially hazardous situations from arising 4 5 System Description General Lamp Information There are a number of different lamps that can be used with the AAnalyst 200 instrument the Lumina Hollow Cathode Lamp HCL and the Electrodeless Discharge Lamp EDL coded and non coded The Intensitron Hollow Cathode Lamp coded and non coded when used with an adapter will function on the AAnalyst 200 instrument All three types of lamps can also be used in the AAnalyst instrument The type of primary source lamp required for your instrument depends on the elements to be determined Either
92. ay the Wavelength dialog You select the desired wavelength in this dialog or touch the numerical entry field and enter the Touch Screens Slit nm desired wavelength Displays the current active slit The slit width and height provides the optimum sensitivity the best signal to noise ratio and good linearity of the calibration curve at the recommended wavelength Touch entry field that displays the spectral width and height of the slit selected to measure the absorption To change the slit touch this field to display the Slit dialog and select the required slit Buttons on Lamp page Set Midscale Setup Instrument Install Lamps You touch this button to set the bar graph to mid scale and perform AGC AIC when you are setting up a lamp The system does this automatically for a lamp when you select Setup Instrument When you have set the lamp parameters touch this button to set up the system with the lamp parameters The system switches the lamp on sets up the optical path prism and grating sets and peaks the wavelength sets the slit and performs an Automatic Gain Control AGC and Automatic Intensity Control AIC You touch this button to display the Install Lamps dialog see below Install Lamps dialog in Lamp page Install Lamps dialog lists the element s lamp type and default current when using coded lamps Bead Install Lamps On Off Elements Current mA Screen 7 4 Install Lamp Dialo
93. bling 9 48 COOP i siaiees eos tine e 6 17 electrodeless discharge e eee 4 9 CLEMENS 2 hois teal iniehiavieed iets 7 9 general information cee 4 6 hollow cathode description 4 6 Intensitron HCL description 4 6 4 8 Installing 2 innen ects de setae sown 6 21 lifespan e a cesbdons viaets 4 10 Lumina HCL description 0 4 7 MAINCENANCE i ledains 4 10 PATAMETETS oerrinne iiie 7 9 replace vss Meek teehee 4 10 9 45 1 6 TEMOVING erer eeno ie egestas 6 24 ON ofi oni tanane a ee 7 9 troubleshooting s es 10 3 types Used ociera 4 6 7 9 uncoded lamp eeeeeeeeseeeeeee 6 30 7 10 M maintenance AUtOSAMPIeL cee eeceeeeeeeeeeeeeeeeeee 9 50 burner chamber disassembling 9 25 burner install 0000cc cece eee 9 26 checklist burner system eee 9 9 checklist general n 9 4 checklist instrument c0cccceeeeeeee 9 5 Cleaning spills eee eeeeeeeeeeeeeeeees 9 4 cleaning instrument eee 9 6 Crain SYStOM eee eee ceeeeeeeeeeeeeees 9 29 drain system flushing 9 30 E Box removing eseese 9 40 E Box replacing 9 42 FIAS enpera a et 9 51 VAMP rien ennnen 4 10 nebulizer performance 64 9 36 Optical system eere 9 5 ordering Parts ee eeecsseceneceteeees 9 54 periodic Checks cee eeeeeeeeeeeeereeeeee 9 7 procedures ein eisai win wes 9 7 replacing drain tubing 9 30 service engineer
94. bulizer and Components Description PE Part Number Nebulizer B315 0520 Spacer B315 0531 Impact Bead B050 5086 Capillary Holder Assembly B315 0525 9 60 AAnalyst 200 User s Guide Drain System Description PE Part Number Drain tube 0250 7987 Deuterium Background Correction Lamp Description PE Part Number Background Corrector D Lamp Assembly B315 0160 Plug Adaptors for use of HCL Description PE Part Number Plug Adapter for use of coded Intensitron N305 0196 HCL Plug Adapter for use of non coded N305 0197 Intensitron HCL Autosamplers Description PE Part Number AS 90plus Autosampler B314 0291 AS 93plus Autosampler B314 0330 MHS Description PE Part Number MHS 15 Mercury Hydride System B314 0760 Holder for Flame heated FIA MHS 15 Cell B300 0350 9 61 Maintenance Spectrometer components Styli pkg 5 N315 0183 Foot switch B315 0627 Ordering Supplies and Accessories Supplies accessories and replacement parts can be ordered directly from PerkinElmer PerkinElmer offers a full selection of high quality atomic spectroscopy supplies through the PerkinElmer e ssentials Catalogue To place an order for supplies and many replacement parts to request a free catalogue or to ask for information call your local PerkinElmer representative or go online to www perkinelmer com 9 62 T
95. cated on the back of the AAnalyst 200 eee ase E ees asa E J translucent blue hose hose PerkinElmer Shelton CT 06484 USA AAnalyst 200 Part Ho Serial No Madein Singapore B FCC Compliance This device complies with Part 15 of the FCC Rules Operation is subject to the following two conditions 1 this device may not cause harmful interference and 2 this device must accept any interference received including interference that may cause undesired Operation black C PerkinElmer s File No LR23329C Cc us EN 35011 Class A Group 1 D Burner Gases Connections For more information see page 5 14 1 9 Introduction Figure D Labels located on the E Box front panel of the AAnalyst 200 EDL2 EDL1 Remote E TRERNET Trigger KEYBOARD SERIAL 1 AUTOSAMPLER PRINTER A AC INPUT POWER Warning Grounding circuit continuity is vital for safe operation of equipment Never operate equipment with DISPLAY grounding conductor disconnected 400 230v IN 50 60 Hz Maximum Power 30 OYA Turn the power switch off and unplug the AC line cord from the AC outlet before loosening the screw WARNING Grounding circuit continuity is vital for safe operation of equipment Never operate equipment with grounding conductor disconnected 1 10 AAnalyst 200 User s Guide Figure E Labels located on the E Box rear p
96. ch Microsoft Excel and select Open from the File menu Navigate through the Open dialog folder to search and open results dat file that was previously copied to the desired directory 18 When the Excel Text Import Wizard window appears select the Delimited option and click Next Text Import Wizard Step 1 of 3 p 2 x The Text Wizard has determined that your data is Delimited If this is correct choose Next or choose the data type that best describes your data riginal data type Choose the file type that best describes your data Delimited Characters such as commas or tabs separate each field Fixed width Fields are aligned in columns with spaces between each field Start import at row 1 File origin windows ANSI Preview of file C WINNT Profiles Administrator Desktop result dat 0 1240 0 1340 0 142 eanO 0 1330SD00 008970RSD 06 7 ample 0060009 25 0203 53 33 PM Screen 7 39 Text Import Wizard Step 1 19 In the second window of the Text Import Wizard select Tab and Space checkboxes The lower pane shows a preview of how the result data will be displayed in Excel Click Next Text Import Wizard Step 2 of 3 i q 21x This screen lets you set the delimiters your data contains You can see how your text is affected in the preview below limiters IV Tab J Semicolon I Comma Vs I other Text qualifier I zl IV Treat consecutive delimiters as one Data preview 97
97. chnique The only difference is in setting up the calibration type Instead of selecting linear for the calibration type you select nonlinear EXAMPLE Determining copper using linear calibration The procedures in this example assume that you have performed the set up procedures in Chapters 3 4 and 5 This example runs a blank 3 standards 2 test samples a reslope standard and 2 more samples The following steps are used in our example 1 Prepare solutions 2 Enter parameters 3 Run the blank 4 Run the standards 5 Run the samples 6 Run the reslope standard T Run the remaining samples Prepare solutions In this example we used a copper lamp and solutions of copper for our determinations However you do not have to use copper For your convenience in making substitutions we have included a table of recommended concentrations for Ag Mg Mn and Pb 1 Prepare about 200 250 mL of 1 v v HNO to use as a blank solution 2 Prepare about 200 250 mL each of three standard in 1 v v HNO ofthe element you want to determine Suggested standard concentrations mg L for five elements are shown in the following table 8 5 Analyzing Samples Table 8 1 Suggested Standards Element Standard 1 Standard 2 Standard 3 Reslope mg L mg L mg L mg L Ag 0 2 0 5 1 0 5 Cu 0 5 1 1 5 1 Mg 0 05 0 1 0 2 0 1 Mn 0 2 0 4 0 6 0 4 Pb 2 5 10 5 3 For samples 1 2 and 3 use Standards 1 2 a
98. cklists ce eesceseceseceseceeeceeeceeeeeseeeeneeenes 9 8 Burner Maintenance Checklist 0 cee ceeeseeeeeeeseeeeeeseeeseecnaecaeceaeeeaeenseeees 9 9 Changing the Air Filter prinesie aiid tits a A anaiei 9 11 Extinguishing the Plame ie cisys ctesieecdietid gaiviiedsiss aia eee E 9 12 Cleaning the Burner Chamber cece esceeseesceceseceseceseceseeeseeeseeeeeeeeaes 9 13 Removing the Burner Door e ee eeceeeeeseeeseeececeeecnseceaeceseeeseeeseeseneesaes 9 15 Replacing the Burner Doot e ee eeeeeseeesceesceececeeecesecesecsaeeeseeeseeeeneeeaes 9 16 Cleaning the Burner System cee eecccsesseeeseecnseceseceaecsseeeseeeseeeseeeeaes 9 17 Cleaning the Burner Head 000 ec cceeeeeeeeseeeneeeeeceaeceseceaeceaeesseeeseeeeneeeaes 9 19 Pre Conditioning a New Burner or Drain Tube 00 eee eeeeeeseeeeeeeeeeeeee 9 21 Removing the Burner Head eee eeeeseeeseeeneecnseceseceseceseeeseeeseeseeeesaes 9 22 Removing the Burner Assembly from the Instrument eee eee 9 23 Disassembling the Burner Chamber uu eeceeeeseesseceseceseceeeceseceeeeeeeeeenes 9 25 Reassembling the Burner System cece eseesceescecseceseceseceeeeseeeseeeeeeeeaes 9 28 Drain System Maintenance ee eesessecsseceseceseceseeseeeeseeeseeeeseeeseeeaaeenaes 9 32 Cleaning the Nebulizer jeini 5 eerie innit dienes Latent 9 36 Replacing Parts Of Wear is i scc stecaestiacs ieseana eee ei 9 45 EB OX e tie o ER A ER O AA A A day iceckavaueten steel 9 46 Maintainin
99. ct the desired elements Use the Clear button to remove unwanted element from the selected list Touch OK Touch the Setup Instrument button on the Lamp page of the touch screen The recommended parameters for that element are automatically set up e The system automatically switches the lamp on sets up the optical path prism and grating sets and peaks the wavelength sets the slit and performs an Automatic Gain Control AGC and Automatic Intensity Control AIC Turn the two alignment controls alternately and in small increments while watching the AA bar graph and the numerical energy readout on Lamp page Align the lamp to obtain maximum energy Turret coded Lumina lamp mount 1 2 Start up the spectrometer but do not ignite the flame If the desired element already appears in the Element entry field box then just touch the Setup Instrument button If you like to select a different element touch the Element entry field box on the Lamp page to display the Element dialog Select the desired element and touch OK e The system automatically switches the lamp on sets up the turret and the optical path prism and grating sets and peaks the wavelength sets the slit and performs an Automatic Gain Control AGC and Automatic Intensity Control AIC 6 31 Operation of the Instrument Turret uncoded Lumina lamp mount 1 2 Start up the spectrometer but do not ignite the flame Touch the Install Lamps butt
100. d in a single user replaceable module called the E Box The operator can just slide the module out from the instrument and replace it with a new one CAUTION Using excessive force and not aligning the module on the track can damage the E Box Removing the E Box 1 2 9 46 Extinguish the flame if lit From the front of the instrument swing open the compartment door and locate the E Box Turn the power switch off and remove the AC power cord from the E Box Disconnect power cord and all cables that are connected to the ports on the front of the E Box Unscrew the door using an Allen wrench Unscrew the flathead locking screw located below the printer connection port Use the E Box handles to pull the module and gently slide it out on the track See the next section to replace the E Box AAnalyst 200 User s Guide Figure 9 15 Removing the E Box from the instrument 9 47 Maintenance Replacing the E Box CAUTION Using excessive force and not aligning the module on the track can damage the E Box 1 Holding on to the E Box with the handles position the E Box to align on the module track 2 Use the handles to gently push the E Box until it is secured in place 3 Screw the locking screw to fully secure the E Box 4 Reconnect the necessary cables to the ports on the module 5 Reattach the compartment door 6 Connect the AC line cord to the E Box and power up the instrument
101. de Lamp Socket Figure 4 3 Drawing of a Lumina hollow cathode lamp Plug The Lumina HCLs are manufactured without cables When they are used with the AAnalyst instrument they are installed simply by sliding the lamp into the single lamp mount or turret Lamp alignment occurs automatically if you have the model with the automatic four lamp turret feature Each Lumina HCL includes a milliampere hour timer in its base This allows you to monitor the lamp usage easily and accurately for Good Laboratory Practices compliance as well as lamp replacement scheduling With a range of 0 to 10 000 milliampere hours the meter measures the number of milliampere hours i e lamp current X hours of operation that your lamp has operated Intensitron Hollow Cathode Lamps The AAnalyst series spectrometers can also be used with the older coded or non coded Intensitron hollow cathode lamps HCLs With the use of the proper adapter cable Intensitron HCLs can be used with AAnalyst instruments System Description If you have a coded Intensitron HCL there is a universal adapter cable N305 0196 to be used with the lamp However lamp coding is lost therefore lamp and element parameters must be set manually when coded HCLs and universal adapter cables are used Intensitron Hollow Cathode Lamp a coded N Co Universal Adapter Cable We for the Coded f Intensitron HC L s N305 0196 Figure 4 4 The Intensitron hollow cathode lamp with un
102. de the required Lumina lamp into the lamp holder and make sure that the integrated socket slides fully home over the receptacle on the lamp holder Align the lamp 3 Close the lamp door Installing and connecting EDLs If necessary assemble the lamp by sliding the lamp driver into the lamp sleeve for the required element Depress the locking pin as the sleeve slides into place and make sure that the locking pin extends through the locating hole in the sleeve Single Coded EDL 1 Open the lamp door 2 Insert the coding plug over the receptacle on the lamp holder NOTE Do not use coding plug for uncoded EDL 6 22 AAnalyst 200 User s Guide 3 Slide the lamp carefully into the lamp holder until it butts up against the end stop inside the holder 4 Connect the lamp cable to an EDL 1 port on the E Box Align the lamp Pi A a P p i i Pad N CO i a Figure 6 12 Assembling an EDL Installing EDLs in the turret version NOTE EDLs may only be installed in positions I and 2 of the turret Refer to Figure 6 15 for the assigned lamp numbers on the turret mount 1 Open the lamp door 2 Insert the coding plug over the receptacle on the lamp holder NOTE Do not use coding plug for uncoded EDLs 3 Slide the lamp carefully into the lamp holder until it butts up against the end stop inside the holder 4 Depending on the lamp position of the turret connect the lamp cable to the corresponding EDL port on the
103. decompose explosively at pressures higher than 103 kpa 1 03 bar 15 psig Always make sure that the acetylene outlet j A WARNING gauge pressure is below this valve AAnalyst 200 User s Guide Setting up the Burner System Summary of the procedure 1 2 Check that the drain trap is filled with water Install the correct burner head for the type of flame that you intend to use air acetylene 10 cm or nitrous oxide acetylene 5 cm See procedures on how to install burner head in the Maintenance chapter If you want to use an impact bead or spacer on the nebulizer make sure that it is correctly installed If you intend to aspirate organic solvents use a yellow color drain tube that is designed for organic solvents Check the burner height Make sure the burner head is balanced at both ends and the burner head is also parallel to the light beam See Adjusting Burner Height later in this chapter Perform the safety checks Ignite the flame NOTE Correct procedures for extinguishing the flame are described later in this chapter 6 5 Operation of the Instrument Assembling the Quick Change Burner Mount Assembly Before the burner assembly can be put into the instrument a few items need to be added or checked The following sections give full procedures to do so Installing the Nebulizer on the Burner Refer to the figure below to install the nebulizer onto the burner end cap Burner Head Bu
104. ded Foam Padding Cardboard Boxed Items as required Carton Sleeve Lie Shipping Carton Base QW Figure 5 1Exploded view of the shipping carton 5 5 Installation Placing the Spectrometer on the Bench Risk of injury through lifting The instrument weighs approximately 49 kg 108 lbs Improper lifting can cause painful and sometimes permanent back injury Use proper lifting postures and or mechanical lifting aids to lift or move the instrument WARNING Prepare to lift the instrument out of the carton You will need two people to do this The bench should be nearby Position a person on each side of the instrument as shown Squat down and place both hands underneath the instrument palms up Spread your hands as far apart as possible against the foam corners while grasping the underside of the instrument With knees bent simultaneously lift the instrument out of the carton as you rise to a standing position Carefully place the instrument on the bench IMPORTANT Use proper lifting posture when taking the instrument out of the shipping carton base Foam Forms Shipping Carton Base Figure 5 2 Lifting the instrument out of the box AAnalyst 200 User s Guide Carton recycling instructions The carton can be folded down for easy storage You can store the carton for future use to transport the instrument or break it down completely and give it to your local recycling center In
105. ds and the end cap When aspirating concentrated samples with complex matrices it is especially important to keep the burner chamber and nebulizer free of sample deposits In addition to regular cleaning it is beneficial to periodically aspirate a dilute surfactant solution such as 0 1 Triton X100 for several minutes to keep the system clean The surfactant solution will encourage constant drainage which is required for obtaining optimum burner system performance When using the AAnalyst nebulizer the impact bead may have to be replaced Also to avoid damage to the impact bead the bead should be removed when cleaning the capillary holder assembly Steps for removing and replacing the bead are included in this instruction document Cleaning the nebulizer 1 After you have taken the nebulizer apart clean the components as follows 9 42 AAnalyst 200 User s Guide Clean the capillary assembly using a mild laboratory detergent solution or a solvent such as isopropanol preferably in an ultrasonic bath Clean the nebulizer body and any other parts that appear dirty in a mild laboratory detergent solution or a solvent such as isopropanol preferably in an ultrasonic bath Rinse all the cleaned components thoroughly with deionized water Inspect the o rings 1 on the capillary assembly and two on the nebulizer body and clean them if necessary in mild laboratory detergent solution followed by a thorough rinsing with deionized w
106. e List Folder Contents Read Write Advanced E Allow inheritable permissions from parent to propagate to this object m O O O O m Cancel Apply Screen 7 27 Properties dialog From the Security dialog highlight Administrators and click Add Click OK Select Full Control for the Administrators Click Apply and then click OK 7 39 NOTE NOTE Touch Screens Network Computer Depending upon the network configuration it may be a Static or a Dynamic network It is best to contact your System Administrator for network setup Network Setup For Dynamic IP Network do the following e Select Obtain an IP address via DHCP option on the Network dialog e Enter the Instrument ID in the entry field box Each AAnalyst 200 instrument must have a unique ID For example AA200_1 1 is the ID number for AA200 instrument 1 The ID can range from 0 255 For Static IP Network do the following e Select Specify an IP address option on the Network dialog e Fill in the entries for IP Address Subnet Mask and Default Gateway Once the Network Setup is completed continue on to Storage Location part of the Network dialog See steps 6 8 of the Stand Alone section for full instructions for setting up Storage Location Certain permissions and restrictions should be set forth by an IT System Administrator Once the shared drive or folder is on the network you can secure it by setting and allowing certain users
107. e sample This entry field allows you to enter the sample dilution AAnalyst 200 User s Guide Analyze Samples Page Manual Continuous Display This window displays the continuous graphics at the top of the screen The display contains a continuous real time plot and a numerical reading for the signal The plot and the numerical value are continuously updated to the current reading The analysis is limited to only one replicate per sample Analyze Blank Auto Scale Graph Printer On Off Analyze Standard Standard 1 10 000 mg L Display Calibration Analyze Sample A ID Sample 001 Dilution 1 000 Screen 7 14 Analyze Samples Page Manual Continuous Display Continuous Graphics Window on the Analyze Page Manual Continous Display The Continuous Graphics window contains a continuous real time plot of absorbance or emission against time The scale for Y axis and real time absorbance default value ranges from 0 00 4 00 absorbance 7 23 Touch Screens Buttons on Analyze page Analyze Blank Analyze Standard Analyze Sample Display Calibration Auto Scale Graph Printer On Off To analyze the blank defined in the method touch this button A green light appears on this button when selected To analyze the standard indicated in the Standard Concentration Box touch this button A green light appears on the button when selected The system analyzes the standard and creates a calibration curve
108. e 1A cylinder of nitrous oxide contains about 14800 liters 523 cubic feet and will typically last for 10 12 hours of burning time Heated regulator Since the nitrous oxide is in liquid form the pressure gauge does not give a true indication of how much nitrous oxide remains in the cylinder until the pressure starts to fall rapidly as the residual gas is drawn off When nitrous oxide is rapidly removed from the cylinder the expanding gas causes cooling of the cylinder pressure regulator and the regulator diaphragm can freeze This can cause erratic flame conditions or in the most extreme case a flashback It is therefore advisable to use a double stage or heated regulator for nitrous oxide to prevent freezing of the diaphragm and a loss of pressure regulation A suitable nitrous oxide pressure regulator is available from PerkinElmer Acetylene supply requirements Warning Acetylene Explosion Hazard y Acetylene can decompose explosively at pressures higher than 103 kPa AN 1 03 bar 15 psig W ARNING e Always make sure that the acetylene outlet gauge pressure is below these values Acetylene can react with copper to form a readily explosive compound e Never use copper tubing or fittings for acetylene gas lines Grade Suitable acetylene ethyne such as atomic absorption grade or welding grade typically has a minimum purity specification of 99 6 with the actual assay being about 99 8 Acetylene is supplied dissolved
109. e and interlock cable will be attached to the drain vessel retainer cap Place the drain vessel in full view on the floor in front of the instrument Never place the drain vessel inside a cabinet 9 29 Maintenance 5 Before connecting the drain tube to the burner assembly pour about 250 mL of water into the free end of the drain tube to fill the drain loop and to activate the drain float 6 Place the hose clamp over the free end of the drain tubing 7 Carefully install the free end of the drain tubing over the drain outlet making sure that the inner lining of the drain tube does not get damaged 8 Use a flat blade screwdriver to tighten the hose clamp 9 Plug the white drain interlock connector into the drain interlock plug on the burner assembly as shown in the photograph below Further procedures for setting up the burner system are described in Chapter 6 Operation of the Instrument To install the burner head 1 Put the burner head back onto the burner chamber while pressing the safety latch tab 2 Position the magnetic strip on the burner head ring around the back of the assembly it should face the ignitor box Release the safety latch Be sure the burner head is fully seated on the chamber A gentle twisting and pushing may be necessary You will know that the burner head is fully seated because the ignitor will swing over the burner 3 Put the burner assembly back into the instrument 4 Check the burner alig
110. e fuel hose They are pointed out in the next figure At this point all three hoses should be already connected to the burner If they are not do so now The next few paragraphs discuss how to check them Nebulizer Clamp f Nebulizer Nebulizer Side Arm Bumer End Cap Auxiliary Oxidant Hose Connector Nut lay Nebulizer la oe Oxidant Hose pa p Figure 6 4 Securing the gas hoses to the burner end cap The first hose is the nebulizer oxidant hose also called the NEB It is connected right after the nebulizer is installed The second gas hose is referred to as the auxiliary oxidant hose AUX It is the other clear hose coming up from under the burner mounting plate and attached to the burner end cap The hose is connected at the factory Confirm that it is connected and that the compression fitting is tight If it is not do the following e Tighten the compression fitting hand tight plus a 4 turn using two wrenches one wrench to hold the nebulizer fitting and the other to turn the compression fitting The third hose connected to the burner is the fuel hose It is the clear tubing attached to the burner end cap Refer to figure Securing the gas hoses to the burner end cap That hose too is connected at the factory Confirm that it is connected and that the compression fitting is tight If it is not tighten it using the procedure that follows e Tighten the compression fitting
111. e gently pulling and twisting the burner head until it comes off the chamber 2 Unscrew the retaining ring Figure below and pull out the burner o ring WS Burner Head Magnetic Strip oe Retaining Ring c Burner O Ring Burner Chamber End Cap O Ring Gasket Plate Guide Pin Burner End Cap Cut outs Nebulizer Clamp Thumbscrews Thumbscrew 1 of 2 Figure 9 7 Exploded view of the burner chamber assembly 3 Lift the nebulizer clamp and carefully rotate the nebulizer arm clockwise slightly slide out the nebulizer Put it to the side 4 Ifyou feel you ll need to completely remove the end cap from the chamber continue with steps 5 7 Otherwise unscrew the four thumbscrews holding the burner end cap and carefully let the end cap hang down you don t have to disconnect any of the hoses Now skip down to step 8 9 25 Maintenance 5 Optional To completely remove the burner end cap disconnect the auxiliary oxidant hose and the fuel hose from the burner end cap using the double wrench method one wrench to hold the nebulizer fitting and the other to turn the compression fitting Burner End Cap Auxiliary Oxidant Line s L gt Compression Fittings Fuel Line Knurled Scr ws Drain Clamp typical 4 places Drain Tube Figure 9 8 Removing the burner end cap 6 Optional Disconnect the drain tube and clamp if they are in place Optional Unscrew the four knurled screws
112. e number pad dialog Enter the required integration time and then touch OK Touch entry field that displays the selected number of replicate measurements The selected number of measurements is performed on each solution blank standard and test sample To change the number of replicates touch this field to display the Replicates dialog Enter the required number of replicates and then touch OK Touch entry field that displays the selected read delay This is the time period that the spectrometer waits before it starts to measure the signal A read delay is typically used to allow the flame to stabilize after a change of solution To change the read delay touch this field to display the Read Delay dialog Enter the required read delay and then touch OK This item allows you to select the information you would like to have printed together with the analytical mean and statistical results You select whether printing should be on or off via the Printer On Off button on Analyze page When the optional autosampler is installed you can choose between manual data display manual continuous graphics display and autosampler Peak Height measures the largest signal during the Read Time after the selected smoothing is applied Peak Area measures the area under a peak in absorbance seconds Smoothing Points uses the Savitsky Golay smoothing algorithm to a group of n data points where n can be 0 5 9 19 and 37 Smoothing is applied t
113. e only regulators tubing and hose connectors approved by an appropriate regulatory agency Arrange gas hoses where they will not be damaged or stepped on and where objects will not be dropped on them Do not refill cylinders Check the condition of pipes hoses and connectors regularly Perform gas leak tests at all joints and seals of the gas system regularly using an approved gas leak detection system The responsible body must carry out appropriate leakage tests necessary for safety on those gas and liquid connections which the operator is directed to assemble during installation normal use or maintenance Check that when the equipment is turned off close all gas cylinder valves tightly at the cylinder Bleed the remainder of the line before turning the exhaust vent off AAnalyst 200 User s Guide Safe use of burner gases The seepage of fuel gas or fuel gas mixture from the burner system the drain system the gas control system or the gas connections constitutes a serious fire hazard If you suspect that the gas box has been damamged for example using the acetylene tank below 5 psi do not use the instrument until it has been inspected by a PerkinElmer Service Representative WARNING e Make sure that there are no breaks or leaks in any of these systems and that all the seals are correctly installed and in good condition e Regularly check for leaks at joints and seals using an approved leak test fluid e When
114. ed You do not need to press forcefully on an active area Note that when you touch an active area various processes may be started in the spectrometer Some of these processes take several seconds Be patient and wait for the process to complete before touching another active area on the touch screen Touch Screens User interface components The user interface components on the touch screen are described below Pages The main displays on the touch screen are termed pages You use the pages to set up your spectrometer and to perform analyses The pages contain Entry fields which allow you to make entries via a dialog Buttons that you touch to start or stop actions or to display a dialog Option Buttons that you use to select an option from a list and Check Boxes that you use to switch functions on or off Dialogs When you touch an entry field or certain buttons a dialog is displayed on the touch screen When you touch a numerical entry field a Numerical Entry dialog containing a numerical keyboard is displayed this allows you to make numerical entry When you touch a parameter entry field a Parameter Entry dialog is displayed you can choose among a number of options When you touch a text entry field a Text Entry dialog containing an alphanumerical keyboard is displayed this allows you to make alphanumerical entries such as user names or file names Tabs 7 4 You use the tabs to select pages either main pages or
115. ed assistance contact the gas supplier or a PerkinElmer service representative Gas hoses and connections can be checked for leaks by applying a soapy solution and checking to see if bubbles appear Be sure the air supply contains less than 20 oxygen Check the source of the gases Lamp Troubleshooting AAnalyst 200 User s Guide Some possible problems are listed below along with probable causes and suggested remedies It is suggested that you use this checklist before contacting PerkinElmer Lamp will not fit in the turret Lamp connector will not fit the plug on the instrument Hollow cathode lamp will not light EDL Electrodeless Discharge Lamp will not light Lamp energy value is too low Lamp energy value is too low continued Possible Cause of Problem If the lamp diameter is smaller than 2 inches it needs a special adapter If the lamp is not a Lumina lamp it needs an adapter If the lamp is not manufactured by PerkinElmer it may need a special adapter cable The lamp may not be plugged into the lamp compartment Instrument is off or not plugged in Lamp not plugged in Lamp worn out or damaged Insufficient lamp current The lamp may not be connected to the EDL power supply The lamp may not be properly aligned The lamp may be starting to deteriorate Possible Cause of Problem The hollow cathode lamp current may be too low Check and or Remedy Use the Small Lamp Ada
116. ee arer aiie i aei 6 5 Installing Solvent Resistant Components in the Burner eee 6 11 Wser Interlaces ceatshed e eie e t ea e er e ena i eae lew es 6 19 Installing Lamps aeeie reiini ie e R RIEA eed 6 21 Switching on the Spectrometer cece eeeessecseceseceteeeeeeeeeeeaeeeseeeaaeenaees 6 25 Safety Checks csiat ssdobes sei soar ar ecaattsenl deat bedaiges ies AEE N 6 26 Using the Background Corrector ceeeeeeseseeeseeeseeeeeeneeeeeeseeeeeeeseeeaes 6 27 Optimization Procedure Ss ieme a aeai iiie 6 28 A onInS Lap esente rencereket EES 6 29 Setting the Burner Height ceennenenin aenea anun ani en 6 33 Teniting the Plame zrno ere a bases a E E dutedens 6 35 Preadjusting the Nebulizer 00 0 eee eeeeseeeseeeneeceseceseceaeceseeeseeeseeeeeeeeaes 6 37 Optimizing the Burner System 0 eee ceseceseceeeceeeeeeeeeeeeeeaeeeaeeenaeenaees 6 39 Rinsing the Burner System ee ee eeseesseeeseeeseecsaeceseceseesseesseesseeeseeesaes 6 43 Chapter 7 Touch Screen User Interfaces rnos eire e era aee EE ati ath erase ines 7 3 Startup Dial Sneen o r eae stole E a eari 7 5 Camp Pae nh ae eree e ae en eee EENES EAEE EE E SEREANTE 7 6 Flame pasene iir eel isk ice tel whod lon eles Meee e Ate cate Aes 7 11 Parameters Paces icciss f3cstitssabesde karese ieie EE EE eE E EE E EESE 7 14 Analyze Page Manual Data Display ee eeseesseceteceteceeeeeeeeeeeeeeeeeenes 7 20 Analyze Samples Page Manual Continuous Display s es 7 23 Analyze Page Autosamplet
117. eived adequate training If the instrument requires servicing only a PerkinElmer service engineer or similarly trained and authorized person must do this If you use the instrument in a manner not specified in the user guides or if you use it for a purpose other than that intended you may damage the instrument or compromise your own or someone else s safety The protection provided by this equipment may be impaired if the equipment is used in a manner not specified by PerkinElmer CAUTION This equipment requires no specified inspection or preventive maintenance to ensure the continuous functioning of its safety features AAnalyst 200 User s Guide Precautions Be sure that all instrument operators read and understand the precautions listed below It is advisable to post a copy of the precautions near or on the instrument WARNING The following precautions must be observed when using the AAnalyst 200 e Be sure that the voltage of the AAnalyst 200 corresponds to the power line voltage used in your laboratory e Never remove the side panels of the AAnalyst 200 without shutting down the instrument and disconnecting the instrument power cord from line power e Only high quality purge gases should be used with the AAnalyst 200 Minimum purity of 99 9 is recommended A high quality filter dryer accessory is recommended for the removal of any moisture from the purge gases 2 5 Safety Practices Hazards with Flame Ato
118. en Enter the word killer exe in the dialog box and touch OK NOTE Allow 10 seconds for Killer exe to terminate all running windows and programs 7 Use the arrow keys on the keyboard to Select Run or touch Run on the touch screen 8 Enter the word repllog in the dialog box and touch OK 7 45 Touch Screens zi xi PK ce Browse Screen 7 34 Run Dialog 9 Follow steps 7 10 from the Connection Setup procedure 10 Follow steps 1 4 of the Downloading procedure 11 Reboot the AA200 instrument 7 46 NOTE AAnalyst 200 User s Guide Importing AAnalyst 200 into Microsoft Excel AAnalyst 200 stores data in flash memory as long as the instrument is powered on Using the procedure below data stored on the AAnalyst 200 can be imported into Microsoft Excel for permanent storage or for custom printing and reporting If Microsoft Office is not available this procedure can also be used to open results using Windows Notepad or Wordpad To import data into Microsoft Excel 1 Insert the AAnalyst 200 Quick Start CD into the CD ROM drive 2 Inthe Main menu of the AAnalyst 200 Quick Start program click on Quit in the lower right part of the window This will exit the AAnalyst 200 Quick Start program 3 Use the Windows Explorer to search for MSASYNC EXE file It is located in the D download directory MSASYNC EXE Where the D is the letter of your CD ROM drive 4 Double click on the MSAS
119. en DES Create Shortcut opie Delete Doc Rename DO Properties dor Screen 7 22 Shortcut menu e Properties folder appear and select Share this folder option 7 35 Touch Screens 44200 Result Data Properties 44200 Result Data fo alow a Screen 7 23 Properties dialog e Click the Permissions button to set users permissions to the shared drive or folder 7 36 AAnalyst 200 User s Guide Permissions for 44200 Result Data 2 x Share Permissions Add Remove Permissions Allow Deny Full Control Change Read Cancel Apply Screen 7 24 Permissions dialog e Click OK and the desired drive folder is now shared sy i Mame O q L Pe AAZ00 Result Data Local Disk C Screen 7 25 Shared folder 8 User Name and Password Enter the user s name and password in the Network dialog If you do not already have a user s name and password follow the procedure below e Select Start gt Settings gt Control Panel The Control Panel dialog appears e Double click Administrative Tools gt Computer Management The Computer Management dialog appears e Inthe directory tree on the left of the Computer Management dialog drill down select System Tools gt Local Users and Groups gt Users e From the Action menu select Action gt New User The New User dialog appears 7 37 Touch Screens e Fill in the dialog completely giving the User Name
120. ensions for the instrument are listed below and shown in the next figure For other accessories refer to the manuals supplied with the accessory The bench should be located near the required electricity and gas supplies Allow additional power outlets for all your accessories A distance of at least 6 inches 153 mm should be surrounding both sides and rear of the instrument for proper ventilation If not possible the bench on which the instrument is placed should be on wheels so that it can be easily moved Accessories Make sure that there is sufficient room near the spectrometer for any accessories For example we recommend that you place the optional flame autosampler and mercury hydride system on the left side of the instrument or on a roll cart in front of the instrument Printer Refer to the manuals supplied with your printer for dimensions The printer may be placed on the bench next to the instrument 3 9 Preparing Your Lab 700 mm 3 10 Figure 3 2 Space requirements for the spectrometer system front view AAnalyst 200 User s Guide 700mm gt 760 mm file h S i Figure 3 3 Space requirements for the spectrometer system top view 3 11 NOTE Preparing Your Lab Exhaust Vent Requirements Exhaust venting is important for the following reasons e It protects laboratory personnel from toxic vapors that may be
121. eously low 10 4 Possible Cause of Problem Corrections may not have been made for reagent blank Ionization enhancement may be present in sample or blank Standard solutions may have deteriorated or may have been improperly made Background absorption molecular absorption light scattering etc may be present This is especially likely to occur below 330 nm or where a high concentration of a refractory matrix is encountered The sample matrix may be less viscous than the standards Matrix interferences chemical bulk viscosity may be present Ionization enhancement may be present in the standard but not the sample Standard solutions may have been improperly made Blank solution may be contaminated Check and or Remedy Zero the instrument while aspirating a reagent blank Add approximately 1000 mg L of an easily ionized salt such as potassium lithium or lanthanum to samples standards and blank Restandardize with a proven standard Use a background corrector or if applicable use a nitrous oxide acetylene flame Remake the standards in the same matrix as the samples or use the method of additions Separate the interferent match the sample matrix in your standards or use the method of additions Add matrix modifiers required to control chemical interferences Add approximately 1000 mg L of an easily ionized salt such as potassium lithium or lanthanum to samples standards
122. er s Guide Cleaning the Burner Head Quick cleaning procedure 1 Extinguish the flame allow the burner head to cool shut down the gases at source and bleed the gas supply lines 2 Open the atomizer compartment door 3 Remove the burner head 4 Carefully work along and through the burner head slot with the cleaning tool provided Do not nick the edges of the slot The cleaning tool resembles a strip of thin metal sheet Do not use other tools to clean inside the burner slot since they may have burrs that could nick the slot 5 Rinse the burner head well with deionized water and make sure that all scrapings are removed from inside and outside the burner head 6 Blow the burner head dry with clean compressed air Wear safety glasses when doing this 7 Reinstall the burner head 8 Close the atomizer compartment door Complete cleaning procedure If the quick cleaning procedure above fails to remove deposits or if you wish to clean the burner head more thoroughly see Cleaning the Burner Chamber on page 9 13 Checking the slot width Over time the burner slot becomes wider due to abrasion The level of abrasion depends on the types of solutions you are aspirating A burner slot that is too wide causes unstable flame conditions and in the worst case may cause a flashback of the flame For this reason you should check the width of the burner slot at regular intervals A set of feeler gauges is required to check
123. er 1 Turn off the spectrometer and turn off all gas supplies 2 Lift the end cap spring clamp 3 Rotate counter clockwise and gently pull the nebulizer out of the burner end cap 4 After removing the nebulizer from the end cap carefully remove the nebulizer gas supply tubing labelled NEB from the nebulizer side arm as follows First loosen the connector nut P N N037 1485 see A Alignment l Keyway Impact Bead NS Structure Nebulizer Th Spacer End View O Rings or A Alignment Key Locking Ring N AN Nebulizer Side GAS Capillary Screw lt 09 Capillary Holder i Nut Gas Supply Connector Nut 9 37 Maintenance e Figure 9 13 Then while holding the nebulizer assembly in one hand rock the gas supply tubing with the other hand while gently coaxing the tubing from the barbs at the end of the nebulizer side arm 5 Remove the impact bead and if using the impact bead spacer remove the spacer as well Handle with care See the next page for instructions 6 Unscrew the capillary tubing Refer to Alignment O Keyway Impact Bead A DI Structure Spacer Nebulizer End View O Rings P Alignment Key NP Locking Ring a G2 Mee Nebulizer Body Adjusting Nut X S Nebulizer Side 6 Spring A ill Capillary Screw f g 5 in O Ring NS ys Capillary Holder Gas Supply Connector Nut 7 Figure 9 13 and loosen and then remove the adjustment nut P N N0
124. er subpage On Parameters page Calibration subpage Select the Calibration Equation 1 For this example select Linear Through Zero Enter mg L for Units On Parameters page Calibration subpage Standard Concentration section 1 Enter the concentration of the first standard for the element that you are determining e g 0 5 mg L for copper Enter the concentration of Standard 2 for the element you are determining e g 1 0 mg L for copper Enter the concentration of Standard 3 for the element you are determining e g 1 5 mg L for copper For the above example we will only be calibrating with three standards Analyzing Samples e Fnter the concentration of the Reslope standard e g 1 0 mg L for copper Parameter entry is now complete Proceed to the next step 4 A E A a I A x aA EN A a PE ISIS Screen 8 2 Parameters page Calibration subpage Analyze samples As measurements are made the results appear on the analyze screen You may view the calibration curve of the analyses at anytime by touching the display calibration button e Touch the Analyze tab to display the Analyze page e Touch the Printer On Off button if you wish the results to be printed 1 Run the blank e Aspirate the blank solution e Touch the Analyze Blank button 2 Run the standards e Aspirate Standard 1 then touch the Analyze Standard button e Aspirate Standard 2 then touch the Analyze Stand
125. eter please take time to read through this self installation guide and become familiar with the steps involved Please make sure your laboratory meets all of the requirements listed in this chapter before you begin to install the system A CD ROM is provided with the spectrometer that contains a video showing the complete installation procedure We strongly recommend that you view this video before you attempt to install your spectrometer Summary of the installation procedure This summary lists the steps you must perform to install the spectrometer 1 2 9 10 Inspect the shipment Unpack the spectrometer Place the spectrometer on the bench Install the touch screen Connect the gas hoses Set up the burner system Install the burner door Install the sample tray Connect the spectrometer to the electrical supply Perform the post installation checks Tools required for the installation You will need the following tools during installation of the spectrometer e small flat bladed screwdriver e two wrenches for gas fittings 5 3 Installation When the Spectrometer Arrives Inspect the shipment Upon receipt of the instrument inspect the exterior of the shipping carton for obvious signs of damage The carton should arrive unopened and undamaged If the carton has been damaged file a claim with the authorized carrier immediately and inform your nearest PerkinElmer office A representative of the sh
126. eter to complete initialization The Lamp page is displayed on the Touch Screen 6 25 Operation of the Instrument Safety Checks Before igniting the flame always make sure that The exhaust venting system for the laboratory is switched on Burner chamber is correctly installed The burner head is correctly installed The burner end cap is secured The nebulizer is installed The correct gaskets are fitted in the burner system The burner drain is connected to the system secured by clamp The drain trap is filled and is operating correctly The door of the atomizer compartment is in the closed position Remove all nearby flammable chemicals Fire extinguisher should be kept nearby Check for chemical residue build up on the burner head slot When igniting nitrous oxide flame warm up the burner head with air acetylene flame for 15 minutes All safety interlocks are correctly closed If the interlocks are not closed one or more of the following may be the cause The burner head the nebulizer or the drain system is not correctly installed The fuel or oxidant pressure is too low The liquid level in the drain trap is either too low or too high 6 26 AAnalyst 200 User s Guide Using the Background Corrector If you have a deuterium background corrector in your AAnalyst 200 you have the choice of performing atomic absorption measurements with or without background correction It is an internally mounted assembly t
127. ex cleaning after use of organic solvents 9 12 disassembly n se 9 25 reassembling seere 9 26 burner door TEMOVING eun i as 9 14 teplacing eni nioena ara 9 15 burner gasket kit 9 52 burner head ACCESSOTICS iiae i o ini 9 52 cleaning ieee ri s 9 19 installeres ain sa eia 9 27 maintenance checklist eee 9 9 TEMO VAN Z sc225s2cpsescsstusassszeeetdoeetsetes 9 22 Slot Width cn sce ete ohn ess 9 19 burner gases required pressures 6 3 burner head installing ioe ensretter deie 6 11 burner system CICAMIN A T 9 17 d sigi ene ei a Bes 4 12 drain System seeeeeeeeeesereeresreesereeses 2 10 OpliMI ZING soapie 6 39 maintenance checklist eee 9 9 reassembling eee eeeeseeeseeeneeeneee 9 26 TINSIN Goose cs Men eel ane Lae 6 43 SEUNG UP si raev a wlio 6 5 burner troubleshooting 0 0 0 0 eee 10 8 C calculated intercept linear 7 19 calibrate analyze samples page eseese 7 26 calibrate stylus tools dialOg niecne niies 7 28 calibration equation s es 7 18 entry on calibration subpage 7 17 calibration subpage eeeeeeeeeees 7 17 diagnostics tools dialOg wo eee ee eeeeeseeereeeneeeeees 7 28 display calibration 0 0 0 0 7 22 7 26 download cee ceeeeeeeeeseeereeeneeeeees 7 41 tools dialog oo eee eeeeeeseeeseeeneeeneees 7 28 Carton recycling eee eeteceseeeeeeeeee 5 7 checklists general maintenance eee eee 9 8 chemicals safely oo nenea i eis
128. for which the lamp is to be used When an RF field is applied to the bulb the inert gas is ionized and the coupled energy excites the vaporized analyte atoms inside the bulb causing them to emit their characteristic spectrum The emission spectra produced is typically much more intense than that from hollow cathode lamps frequently tenfold larger or more Lamp Installation When you first receive your instrument there is no lamp source installed For initial lamp installation details see Chapter 6 Operation of the Instrument in this manual If you need to replace an existing lamp see Chapter 9 Maintenance later in this manual contains the various lamp replacement procedures System Description Lamp Alignment Refer to Chapter 6 Operation of the Instrument in this manual for the procedures to align a lamp in an AAnalyst instrument Lamp Maintenance and Cleaning There are really no maintenance procedures for any of the PerkinElmer hollow cathode lamps If you notice fingerprints on the window of your lamp wipe them off with a soft dry lint free cloth Do not use chemicals or water See the section below regarding lamp life and when to replace them Lamp Life Both hollow cathode and electrodeless discharge lamps have a finite lifetime Electrodeless discharge lamps typically last longer than hollow cathode lamps for the same element If while aligning a lamp you are not able to obtain a satisfactory energy value this may
129. fting it from the nebulizer s body assembly Installing Spacer The nebulizer assembly can be used with or without the spacer Maximum sensitivity for Air Acetylene elements can be achieved without the use of the spacer The addition of the spacer reduces the amount of sample delivered to the flame It is recommended to use the spacer for all elements analyzed with the nitrous oxide acetylene flame and for elements which are air acetylene flame sensitive such as calcium chromium and gold When analyzing some complex sample matrices it may be desirable to add the spacer to reduce chemical interferences To Install Spacer 1 Hold the impact bead by its base only 2 Rotate it approximately 1 8 turn counter clockwise before carefully lifting it from the nebulizer s body assembly 3 Place the spacer onto the back of the nebulizer and replace the impact bead 4 Rotate the bead 1 8 turn clockwise to lock the bead in place Impact Bead N Spacer O Rings oO Nebulizer Body Nebulizer Side Arm Figure 9 14 Installing Spacer onto the Nebulizer 9 40 AAnalyst 200 User s Guide Adjusting the Nebulizer for Maximum Absorbance Adjust the nebulizer to achieve maximum absorbance as follows 1 10 Ignite the flame Refer to the procedure for igniting the flame in Chapter 6 Operation of the Instrument Set up the spectrometer for the determination of copper magnesium or another element which h
130. g Four Lamps On Off Elements Type Current mA 7 8 Screen 7 5 Install Lamp Dialog Single Lamp AAnalyst 200 User s Guide Parameters on Install Lamps dialog On Off Elements Type Current Lamps can be turned on or off by using the touch entry field box to check uncheck lamps and touch the OK button Coded lamps the instrument detects the element s and automatically fills the Elements entry box Uncoded lamps the atomic symbol for the element must be entered manually Touch the Element box lightly for the Select Element dialog This shows the type of lamp installed The instrument automatically fills in this entry for coded lamps To change the lamp type touch this field to display the Type dialog and select the required lamp type HCL Hollow cathode lamp EDL Electrodeless discharge lamp lamps can be connected to EDL position 1 or position 2 This is the operating current for the lamp The system sets the recommended current To change this use the touch entry field to view the touch number pad dialog Use the touch number pad to enter the value For uncoded lamps enter the atomic symbol in the Elements entry field and the system will set the current You may change this value if necessary When the lamp is nearing the end of its useful life you may want to use a higher current the maximum permitted current is shown on the label of the lamp Entering analytical parameters
131. g the Acetylene Supply esesssssesseesesessreesesrrssrrsrssresresressesreses 9 50 R placing the Lamps 3 scsec seeta sate iedesti sities ceted a a a 9 51 Replacing the Deuterium Arc Background Corrector Lamp 008 9 52 AS 90plus and AS 93plus Autosampler Maintenance eee 9 56 MHS 15 Mercury Hydride System Maintenance 9 57 Replacement Parts and Accessories eeeeeeeeeseeeseeeeeceeeceaeceaeceaeeeneeeaes 9 60 Chapter 10 Troubleshooting IMO MUCHO Senare eena aeae PEE REE ATENE ENE 10 3 Flame Analysis Troubleshooting eeeeeseeeeesereesesrreserrresresrrsresrrsrresesees 10 4 Flame Burner Troubleshooting eeeeseceesereerrereesesrisserrresrerrssresresreesesees 10 8 Lamp Troubleshooting esessseeseeeeesesessereresresrrsrtsresressesrissresrssrenresressesees 10 11 Troubleshooting Deuterium Background Corrector Problems 10 13 Index Introduction 1 AAnalyst 200 User s Guide About This Manual For complete safety label information see AAnalyst 200 Quick Installation and Setup Guide 0993 6593 This User s Guide is divided into the following chapters Chapter 1 Introduction This chapter contains a brief introduction on the instrument the conventions and warnings used in the manual Chapter 2 Safety Practices Important safety information for the AAnalyst 200 is provided in this chapter Chapter 3 Preparing Your Laboratory The preparation of your laboratory needed for the AAnal
132. groups rights to the shared drive folder 7 40 AAnalyst 200 User s Guide Download To download new software firmware it is necessary to first establish a connection between a computer and the AA200 instrument using Microsoft ActiveSync program Download Requirement e Computer running Windows NT 2000 or XP e RS 232 female to female Serial Cable e Microsoft ActiveSync file msasync zip from QuickStart CD 0993 6637 Download folder Follow the procedure below to download software firmware Connection Setup 1 Install Microsoft ActiveSync if not already installed 2 Follow the setup wizard from the Microsoft install shield Microsoft ActiveSync Set Up Microsoft ActiveSync 3 5 Before you can exchange information between your mobile device and this computer you must set up ActiveSync This setup wizard will guide you through Installing the ActiveSync program on this computer Setting up your mobile device Note It is strongly recommended that you exit all Windows programs before continuing with this setup wizard Click Next to continue with the setup process Click Cancel to quit setup lt Back Cancel Help Screen 7 28 Microsoft ActiveSync Install Shield 7 41 Touch Screens 3 Pause at the Get Connected window and physically connect the RS 232 serial cable from the E Box to the computer e Connect RS 232 serial cable to the serial 1 of the E Box e From the E Box run the RS
133. hat provides simultaneous correction for molecular absorption and light scattering The spectrometer uses a deuterium arc lamp to correct for background absorbance caused by non atomic species in the atom cloud When the deuterium arc background corrector is used two alternating sets of measurements are made one with the primary source and a second with background corrector source The primary source measures a combination of background and atomic absorption The continuum source measures only the background The difference between the two measurements yields the atomic absorption A deuterium arc source is used for maximum wavelength coverage and intensity The AAnalyst 200 can accurately handle combined atomic plus background absorption signals as large as three absorbance units The background corrector is internally installed with its power supplied from the instrument Power to the source is automatically and continuously adjusted to be in the optimum range for operation The deuterium arc lamp is easily accessible allowing convenient replacement of the lamp by the users 6 27 Operation of the Instrument Optimization Procedures Before you calibrate the spectrometer and begin analyses you must optimize the spectrometer to obtain the best conditions for analyzing the requested element in your samples You can optimize e The lamp You must align the lamp in the optical path so that maximum radiant energy passes to the detector
134. he drain tubing and pour approximately 250 mL of water into it until you hear the water start to drip into the vessel 6 14 AAnalyst 200 User s Guide mie o Spiral Wrap Drain Interlock Cable a Ei E Connector at Burner i Interlock Cable x Drain Tubing 3 Drain interlock Float Switch Assembly Figure 6 7 Installing the burner drain system 6 15 Operation of the Instrument 3 Now attach the free end of the drain tubing outlet on the burner end cap Tighten the drain clamp Burner End Cap Burner Assembly Drain Interlock Plug Drain Interlock Connector Interlock Cable Figure 6 8 Connecting the drain tubing and drain interlock cable 4 Finally you need to connect the drain interlock cable Plug the drain interlock connector into the drain interlock plug located on the burner assembly as shown above 6 16 AAnalyst 200 User s Guide Adding water to the Drain Float Assembly Enough water must be present in the drain system to fill the drain loop and to activate the drain float assembly If not carry out the procedure below 1 Loosen the drain clamp and remove the drain tubing from the drain outlet on the burner end cap see Figure 6 8 2 Pour about 250 mL of water into the drain tubing 3 Reconnect the drain tubing to the burner end cap
135. holding the end cap to the burner chamber and carefully remove the end cap 8 Remove the flow spoiler from inside the burner chamber 9 26 AAnalyst 200 User s Guide Unscrew the two thumbscrews holding the burner chamber and plate to the burner assembly one thumbscrew can be seen under the burner chamber in Magnetic Strip Retaining Ring C Bumer 0 Ring Burner Chamber End Cap O Ring Gasket j Plate Burner End Cap Guide Pin Cut outs Nebulizer Clamp Thumbscrews Thumbscrew 1 of 2 Flow Spoiler Six O clock Position 9 Figure 9 7 Exploded view of the burner chamber assembly Lift the burner chamber and plate from the assembly 10 Clean the chamber Place parts in an ultrasonic cleaner and let them soak in a detergent solution in the machine until they are completely clean 11 Remove rinse with deionized water and allow to dry 9 27 Maintenance Reassembling the Burner System After you have completed maintenance procedures reassemble the burner system as given below To reassemble the burner chamber 1 Before you reassemble the burner system verify that the o rings are in good condition If an o ring appears damaged replace it CAUTION Lightly lubricate the surface of the o rings Too much Apiezon grease on the o rings will affect instrument performance 2 Screw the two thumbscrews holding the burner chamber and plate to the burner assembly 3 Place the flow spoiler
136. hollow cathode or electrodeless discharge lamps may be used Hollow cathode lamps HCLs are excellent for most elements however there are a number of difficult elements for which an improved light source is desirable Electrodeless discharge lamps EDLs are more intense than the HCLs Most EDLs provide better lamp life stability and in some cases better sensitivity The 3 types of lamps that can be used in the AAnalyst 200 are listed e the Lumina hollow cathode lamp HCL e the coded Electrodeless discharge lamp EDL System II e the coded and non coded Intensitron hollow cathode lamp HCL with adaptors The basic AAnalyst 200 instrument has a mount for a single lamp It can however be purchased with an automatic four lamp turret An Explanation Hollow Cathode Lamps HCLs The specific determination of one element in the presence of others is possible with the use of special light sources and careful wavelength selection in a spectrometer A single element lamp emits specific wavelengths of light for the element from which the cathode is constructed There are single element lamps for all elements commonly measured by atomic absorption Hollow cathode lamps HCLs are ideal for determining most elements by atomic absorption spectroscopy Refer to figure below The basic components of an HCL are a glass cylinder filled with an inert gas argon or neon at low pressure an anode a cathode and a quartz window with a graded seal to
137. ht Spot White Card Bumer Slot Burner Head Figure 6 16 Locating the radiation beam above the burner If the burner is too high so that it obstructs the radiation beam lower it with the vertical alignment control If the radiation beam is not approximately centered over the burner slot adjust the burner position with the horizontal alignment control 6 33 Operation of the Instrument Figure 6 17 Burner alignment controls 1 Touch the Flame tab to display the Flame page 2 Lower the burner with the vertical alignment control so that the burner head is well below the radiation beam 3 Touch the Auto Zero Graph button to zero the absorbance display 4 Raise the burner with the vertical alignment control until the display indicates a slight positive absorbance reading 0 002 to 0 004 absorbance 5 Very slowly lower the burner with the vertical alignment control clockwise until the absorbance reading returns to zero 6 Finally rotate clockwise the vertical alignment control an additional half turn 6 34 AAnalyst 200 User s Guide Igniting the Flame WARNING u gt A Warning Flammable Gases Fire and Explosion Hazard Before you ignite the flame setup your spectrometer and burner correctly and observe all the safety precautions described in your spectrometer guide Warning UV Radiation Risk of Eye Damage The flame especially the nitrous oxide acetylene flame may emit UV radiation which ca
138. ibed in this chapter If additional maintenance is required contact a PerkinElmer Service Engineer Before using any cleaning or decontamination methods except those specified by the manufacturer users should check with the manufacturer that the proposed CAUTION method will not damage the equipment Maintenance General Maintenance Checklist The following checklist describes general maintenance procedures e For safety reasons and to avoid contaminating new samples you should ensure that the work area is kept absolutely clean This is especially important when working with toxic substances and when measuring trace amounts of any elements e Clean up spills immediately using a spill clean up kit approved by your organization In accordance with safe laboratory practices spilled material should be cleaned up and disposed of properly taking into consideration the following WARNING e location and size of the spill e chemical and physical properties of the material e hazardous properties of the material and types of personal protective equipment that might be needed AAnalyst 200 User s Guide Instrument Maintenance Checklist Flame should be turned off while performing the instrument maintenance checklist CAUTION To properly maintain the spectrometer instrument do the following as required e Clean the exterior of the instrument e Inspect and clean any fans and filters e Monitor tank pressure
139. ied with the AAnalyst 200 and accessories before you start working with the instrument Carefully read the safety information in this chapter and in the other manuals supplied When setting up the instrument or performing analyses or maintenance procedures strictly follow the instructions provided Safety Practices Working Safely with the AAnalyst 200 Built in safety This instrument complies with international standards governing the safety of laboratory equipment In routine use the instrument poses virtually no risk to you If you take some simple common sense precautions you can maintain the continued safe operation of the instrument Safety interlocks PerkinElmer provides a number of safety interlocks on its instruments that monitor such things as door locks gas pressures and the temperatures of various components Do not attempt to defeat these interlocks you may compromise your own or someone else s safety Correct use of the instrument Before you install or use your instrument and in order to get the best results you should be familiar with all of the instruments in the system and know how to operate them You should also be aware of the safety procedures in force in your laboratory especially those concerning atomic spectrometry instruments Consult the guides supplied with the instruments before you start The persons who use this instrument and perform the routine maintenance must be suitably qualified and have rec
140. iew the status of safety interlocks Interlocks N20 Pressure C2H2 Pressure Nebulizer Interlock Burner Head Interlock Drain Interlock Update Screen 7 8 Interlock Dialog SENN NOTE f air acetylene is used in place of N20 the MN 0 pressure interlock will be ignored and flame will light 7 13 Touch Screens Parameters Page You enter the analytical parameters on the Parameters page This page comprises two subpages Spectrometer subpage e Calibration subpage Spectrometer subpage You enter spectrometer related parameters on this page This is always the first page shown when you touch the Parameters tab A IN TN IN N IN IN N IN IN IN N IN IN IN IN IN IN N IN T D Screen 7 9 Spectrometer Subpage MHS Technique 7 14 AAnalyst 200 User s Guide IN 2 A IN N A I IN IN IN IN N my A N T A D IX IN A z Screen 7 10 Spectrometer Subpage Flame Technique 7 15 Touch Screens Items on this page Integration Time sec Replicates Read Delay sec Print Sample Handling Measurement MHS only Smoothing Points MHS only Peak Plot Scale MHS only 7 16 Touch entry field that displays the selected integration time This is the time period over which the spectrometer takes a measurement The longer the time the greater is the level of signal integration To change the integration time touch this field to display th
141. ikely to expose live parts Even when the power switch is off high voltages can still be present Capacitors inside the instrument may still be charged even if the instrument has been disconnected from all voltage sources The instrument must be correctly connected to a suitable electrical supply The supply must have a correctly installed protective conductor earth ground and must be installed and checked by a qualified electrician before connecting the instrument Any interruption of the protective conductor earth ground inside or outside the instrument or disconnection of the protective conductor terminal is likely to make the instrument dangerous Intentional interruption is prohibited When working with the instrument e Connect the instrument to a correctly installed line power outlet that has a protective conductor connection earth ground e Do not operate the instrument with any covers or internal parts removed e Do not attempt to make internal adjustments or replacements except as directed in the manuals e Disconnect the instrument from all voltage sources before opening it for any adjustment replacement maintenance or repair If afterwards the opened instrument must be operated for further adjustment maintenance or repair this must only be done by a PerkinElmer Service engineer or similarly authorized and trained person e Whenever it is possible that the instrument is no longer electrically safe for use m
142. in acetone propan 2 one to prevent explosive decomposition You should not use acetylene that is dissolved in any other solvent Experience indicates that solvents can be carried through the regulator with the acetylene and can weaken to the point of rupture the walls of the tubing carrying the acetylene to the burner causing a potential hazard Cylinder information A size 1A acetylene cylinder contains about 8500 liters 300 cubic feet of acetylene and usually lasts about 30 hours of burning time with an air acetylene flame With a nitrous oxide acetylene flame the same size cylinder will last about 10 hours 3 18 AAnalyst 200 User s Guide Flash arrestor PerkinElmer recommends the use of the Flash Arrestor P N N930 0068 The flash arrestor provides a positive gas shutoff by checking the reverse flow under all conditions It also stops the gas supply when a flashback occurs The flash arrestor can be directly connected to the acetylene fuel line Piping tubing fittings Use galvanized iron steel or wrought iron tubing Never use copper tubing with acetylene Joints may be welded or made up of threaded or flanged fittings typically stainless steel or aluminum or brass composed of less than 65 copper Rolled forged or cast steel or malleable iron fittings may also be used Cast iron fittings cannot be used safely for acetylene lines Safe use of acetylene e Periodically check for the presence of acetylene in the laboratory
143. ing Organic Solvents It is often beneficial to lower the nebulizer uptake rate when aspirating organic solvents The normal nebulizer uptake rate is typically 6 8 mL min By reducing the uptake rate to 2 4 mL min it is usually possible to operate with a leaner blue flame than is possible with higher nebulizer uptake rates This leaner flame typically provides improved precision particularly when aspirating xylene To adjust the nebulizer uptake rate unlock the nebulizer locking nut and rotate the nebulizer adjustment nut until you locate a position which provides reduced sample uptake Then lock the nebulizer locking nut NOTE The uptake rate is easily measured by using a graduated cylinder 9 41 Maintenance Maintaining Optimum Nebulizer Performance To maintain optimum nebulizer performance you must periodically clean the capillary assembly and occasionally replace the capillary sample tubing See E Alignment Keyway Impact Bead Nebulizer Th Spacer End View O Rings ae CO to Alignment Key Locking Ring vee ae N Capillary Screw G ae O O Ring Capillary Holder Gas Supply Sipe Connector Nut Nebulizer Body __ Nebulizer Side Arm Figure 9 13 for an exploded view of the nebulizer Also the nebulizer is only a part of the overall burner system For optimum burner system performance it is important to periodically clean the nebulizer burner chamber burner hea
144. ing organic solvents Clean the burner chamber before you switch to aqueous solutions Empty the drain vessel and dispose of hazardous solutions If you are analyzing samples containing high concentrations of copper silver or ercury Thoroughly flush the burner chamber and drain tube immediately after ompleting such analyses Empty the drain vessel and dispose of hazardous solutions Burner head Inspect the burner head for deposits before igniting the flame The burner should provide an even flame over the length of the burner slot An uneven flame may indicate that the slot needs cleaning See page 9 19 for cleaning procedure heck the width of the burner slot periodically Nebulizer f there is an obstruction in the nebulizer clear it using a copper cleaning wire Flush the drain system thoroughly at the end of each working day by pouring water down the neck of the burner chamber Drain trap Periodically remove the drain trap and clean Inspect the drain tube regularly for wear and or chemical attack Replace it if it has deteriorated Drain vessel Empty the drain vessel regularly Do not allow it to fill with corrosive toxic or organic solutions Dispose of hazardous solutions properly ain ain ain O rings heck the condition of the o rings regularly burner end cap o ring o ring in neck of burner chamber three o rings on the nebulizer as hoses heck the gas hoses regularly for leaks particularly at the fittings using a
145. inside the burner chamber 4 Screw the four knurled screws holding the end cap to the burner chamber and carefully attach the end cap 5 Connect the drain tube and clamp 6 Connect the auxiliary oxidant hose and the fuel hose to the burner end cap using the double wrench technique method one wrench to hold the nebulizer fitting and the other to turn the compression fitting 7 Carefully slide the nebulizer into the end cap and lock into place with the nebulizer clamp 8 Place the burner o ring into the burner chamber and screw on the retaining ring 9 Press the safety latch on the ignitor box while gently pushing and twisting the burner head onto the chamber 9 28 AAnalyst 200 User s Guide Bummer Head Magnetic Strip Retaining Ring Burner Chamber Plate Guide Pin Cut outs End Cap O Ring Gasket Burner End Cap Nebulizer Clamp Thumbscrews Thumbscrew 1 of 2 Flow Spoiler Six O clock Position Figure 9 9 Exploded view of the burner chamber assembly To install the burner in the spectrometer Guide the burner assembly into the tracks of the atomizer compartment Push the burner assembly in so that the rear gas fittings line up with the gas connectors at the back of the atomizer compartment Push the burner assembly fully in until it clicks into place Pull the lever forward and insert the locking pin to lock the burner assembly in place Locate the drain vessel The drain tub
146. instrument touch screen AAnalyst 200 The next figure shows a block diagram of how the AAnalyst burner system flows from the gas supplies to the gas box to the burner hardware itself and out to the drain vessel 4 13 System Description jesse ueq aqn Areyideo ajdwes JOZIINQEN dep pug SS E Ajquessy Jouing wuy 10 1U 6 jens JUepIXO Aye lixny O u wnyysu o mm yeusajul xog seg JUEPIXO J9ZI INGON 8GZ0 Z700 Alquiessy 8SOH PIXO SNOIN A0EZ 67 E0 E0E0 AZLL v0Z0 E0E0 eyeey uUl ING sapnjoul soyejnBay PIXO SNOIN yueL P pPIXO SNOIN j 86 L O 6N 494 4 U97994 11 10 2G90 Zr00 1 414 194 AY 1990 2900 Sr A quiessy 8SOH uoIy y 6550 2900 Alquiessy aso aua Ajooy 8900 0 6N Jo seuy use 9010 0 0 uoN ang JoyeinBay u j 90y oO Ul JI yoelg yuel aue Ajooy SER 7 ul aua Ajaoy pay e7 EAZ 01S 10006 ONWDO Z S1Z 0660 eIdepy lt Bums uolsseidwoy UIQL G Buy uoisseidwoy UL QL G O Odlg Ul p 976 0660 JOPSBUUND JLN A ddns Jy Figure 4 8 Block diagram of the complete burner system 4 14 AAnalyst 200 User s Guide The Burner Head All the burner heads are made from titanium The 10 cm air acetylene burner head is standard with the AAnalyst instruments All the available burner heads are listed next in numerical
147. ion 5 24 exhaust Capacity oenen estan sea nen 3 13 VENU atiota e leat ee Mae 3 12 Vent Kitisescctisetiiesiate ersi t sbi ieceat 3 14 explosion acetylene fess paee ha eet ees 3 18 extinguish flame see eeeeeeeeeeeeeeeees 6 43 F figures after decimal cesses 7 17 first sample location essees 7 26 flame CEMMISION 2 0 0 0 cece eeeeeeeeeeeeeeeree es 7 7 Index flame on off b tt eere R EEEN 7 13 flame page description seeeseeseeeesereeerrersreee 7 11 fittings acetylene supply 0 0 eee eeeteceeteeeees 3 19 flame TOINE 2 sce Sey sereaierbec dace inecedsboacetaesotcc 6 35 troubleshooting 10 8 flame atomization safe operation of the flame 2 10 safe use of burner gases eee 2 17 flash arrestor Acetylene or en e e Aes 3 19 flashback a E EET 3 17 causes 10 10 foot switch COnnection sssesseeseeseseesesesesee 5 24 5 26 G gas ACELVIENE nennen er noni 3 18 COMPTESSEM eissi iiseaetniseiiei tens 2 14 COMMECHNG neii i 5 14 CVLMNASTS iseina esi ends 2 15 recommMendations csesseeeseceseees 3 15 SUpp LY erste Hassteesh aiadiceee a genes 3 16 CESCHIPUIOM ssiey ies cscensse spect dereeestacecansenee 4 16 gas flows 0 0 5 00010400 ose 6 41 gases burner safety s oeeie aeoaea e E 2 17 H hazards ACELYIENE s tiscsts Laced insets 3 18 acetylides oiran eieiei tens 2 7 Cyanide solution eeeeeeeeereeeereee 2 7 flame atomization eee cece
148. ip the exhaust end of the system with an exhaust stack to improve the overall efficiency of the system Make sure the length of the duct that enters into the blower is a straight length at least ten times the duct diameter An elbow entrance into the blower inlet causes a loss in efficiency Position the discharge outlet away from open windows and inlet vents Exhaust capacity The system should provide a flow rate of 5600 8400 liters minute 200 300 cubic feet minute Measure the flow rate at the inlet to the hood with a suitable air flow meter to ensure that the system is drawing properly Provide make up air to the laboratory in the same quantity as is exhausted An airtight laboratory will cause a loss in efficiency in the exhaust volume Blower information The required capacity of the blower depends on the duct length and the number of elbows or bends used to install the system If an excessively long duct system or a system with many bends is used a stronger blower may be necessary to provide sufficient exhaust volume The blower should be located at least 4 meters 13 1 ft and not more than 6 5 meters 21 3 ft from the inlet directly above the instrument and should exhaust to the atmosphere or into a considerably wider exhaust duct 3 13 Preparing Your Lab In many countries PerkinElmer offers an accessory blower and vent kit that will fulfill the exhaust requirements for all atomic spectroscopy instruments or your
149. ipping carrier must be present for insurance purposes How to unpack the spectrometer Carefully read these instructions before you unpack the AAnalyst 200 to avoid damaging the instrument The AAnalyst 200 is shipped in a single carton The carton contains the instrument in the lower portion of the box with an inner tray designed to hold items in the upper portion of the box The touch screen atomizer compartment door drain bottle sample shelf user guides and small parts are contained in the inner tray 1 Place the instrument carton on the floor in front of the bench on which the instrument will be placed 2 Cut the two bands that hold the carton together lift off the top of the carton 3 Pull out the two foam pieces that secure the instrument in the box 4 Remove the three small cardboard boxes from the carton 5 Lift up and remove the carton sleeve the sides of the box 6 Next remove the protective wrapping around the instrument not shown 7 Prepare to lift the instrument out of the carton You will need two people to do this The bench should be nearby The instrument weighs 49 kg 108 Ib Use proper lifting posture when lifting the instrument out of the carton Be aware that most of the weight is located at the right front corner of the instrument It will want to tip forward when it is lifted out of the carton so be prepared to support that corner WARNING AAnalyst 200 User s Guide Shipping Carton Top Mol
150. isplay the Analyze page Touch the Printer button if you wish the results to be printed Check printer function the printer already maybe on 1 Aspirate the blank 2 Touch Analyze Blank button 3 Aspirate Standard 1 and then touch the Analyze Standard button After a standard is analyzed the next standard concentration is automatically incremented in the standard entry field box You have the option of using the automatically filled entry or you may select a different standard concentration to be analyzed by using the standard touch entry field box The dialog displays a list of standard concentrations that you can choose from 4 Aspirate Standard 2 then touch the Analyze Standard button 5 Aspirate Standard 3 then touch the Analyze Standard button 6 To view the calibration curve touch the Display Calibration button 7 Aspirate sample 1 then touch the Analyze Sample button After a sample is analyzed the next sample ID is automatically incremented in the sample entry field box You may enter a sample number by touching the sample entry field box to use the keypad 8 Aspirate sample 2 then touch the Analyze Sample button Analyze Blank Printer OVON 53 Analyze Standaed Display Calibrason Analyze Sampie 2 ID Sarrple 002 Daton fi 000 Screen 8 8 Analyze page 8 14 AAnalyst 200 User s Guide Automated Flame Analyses If you selected Autosampler for Sample Handling on Spectromete
151. ition 7 28 This button displays the diagnostic dialog used to make sure that your instrument and its accessories have been installed properly and are functioning properly This button displays the Recommended Conditions dialog which shows recommended analytical conditions for determining the active element The data tab displays the recommended setup and diagnostic parameters of wavelength slit width relative noise characteristic concentration sensitivity check and linear to mg L The remark tab displays special conditions about the element that you are determining To view a different element for recommended conditions the element in lamp page must be changed This button displays the Network dialog that is use to setup a network connection between the instrument and a stand alone or a network computer Once a network connection is established all the analyses result data will automatically be saved Touch this button to run a system utility to recalibrate the touch screen if the screens are not responding properly to your touch Touch this button to print the current active method This button is to be used by service engineers This button is to be used to upgrade software Touch this button to set time zone daylight saving date and time Touch this button to format date and time display Touch this button to change technique Touch this button to show a plot of the most recent wavelength peaking operation fo
152. iversal adapter cable N305 0196 Non coded HCLs can also be used with the appropriate adapter cable N305 0197 however lamp and element parameters must be set manually when non coded lamps are used ia Intensitron S Adapter Cable Hollow Cathode for the Non coded Lamp Intensitron HCL s non coded N305 0197 Figure 4 5 The noncoded Intensitron hollow cathode lamp with adapter cable N305 0197 4 8 AAnalyst 200 User s Guide Electrodeless Discharge Lamps EDL System Il While hollow cathode lamps are an ideal source for determining most elements by atomic absorption for volatile elements an electrodeless discharge lamp EDL is recommended instead EDLs provide greater light output for improved detection limits and precision along with increased sensitivity and working curve linearity EDLs also have a longer life than corresponding hollow cathode lamps For certain elements such as arsenic and selenium EDLs will also provide improved sensitivity Lamp Sleeve Lamp Driver Locking Pin a Note This cable connects to the Lamp1 or Lamp2 receptacle on the back of the EDL Power Supply er a Note This coding plug is not Use this coding plug used with the AAnalyst with the AAnalyst Instruments Instruments Figure 4 6 An Electrodeless Discharge Lamp EDL An EDL consists of a quartz bulb under an inert gas atmosphere containing the element or a salt of the element
153. l against them Locate gas cylinders away from heat sources including the direct rays of the sun and away from ignition sources and readily ignitable substances such as gasoline oil or combustible waste Compressed gas cylinders should not be subjected to temperatures above 52 C 126 F Locate all gas cylinders only in a vertical position fastened securely to an immovable bulkhead or a permanent wall Move cylinders with a suitable hand truck after making sure that the valve cap is securely in place and that the cylinder is properly fastened to the hand truck Do not attempt to refill gas cylinders 3 15 Preparing Your Lab Two types of flame are commonly used for atomic absorption analyses with flame atomization the air acetylene flame and the nitrous oxide acetylene flame The specifications and requirements for the burner gases are given below Purity Outlet Gauge Pressure Bar rtm Frm ain Pma Pain Pmax Acetylene ethyne C2H2 99 6 atomic 1 0 12 14 absorption grade in acetone propan 2 one oxygen lt 20 particle 300 400 3 0 4 0 44 58 free oil free water free INitrous oxide dinitrogen 300 400 3 0 4 0 44 58 monoxide N20 Never set the outlet pressure to a value exceeding the maximum pressure Pmax Warning Acetylene Explosion Hazard Acetylene can decompose explosively at pressures higher than 103 kPa 1 03 bar 15 psig WARNING Always make sure that the ace
154. l with water Dispose of hazardous or corrosive solutions properly and observe local codes concerning the effect of the waste on the environment Dispose of hazardous or corrosive solutions properly and refer to your local safety regulations for proper disposal procedures 9 13 Maintenance Cleaning the burner chamber after aspirating solutions containing Cu Ag or Hg If you have aspirated high concentrations of copper silver or mercury solutions into an acetylene flame unstable acetylides may have formed in the burner chamber If permitted to dry these compounds may explode 1 2 5 Aspirate dilute acid 1 v v HCI solution for 5 minutes before turning off the flame Extinguish the flame and allow the burner head cool Remove the burner head Pour about 500 mL of deionized water slowly through the neck of the burner chamber to thoroughly flush the chamber and the drain system Empty the drain vessel NOTE Dispose of hazardous or corrosive solutions properly and refer to your local safety regulations for proper disposal procedures 9 14 AAnalyst 200 User s Guide Removing the Burner Door Refer to the figure below when removing the burner door 2b enough to tilt the top of the door away from the upper door bracket Exert enough upward pressure on the lower left corner of the door Swing the door open to about the 45 degree position Lower the door free of the
155. layed this allows you to make alphanumerical entries such as user names or file names Tabs e You use the tabs to select pages either main pages or pages within dialogs 6 20 AAnalyst 200 User s Guide Installing Lamps Three versions of the AAnalyst 200 spectrometer are offered e The first version is designed to operate with a single PerkinElmer Lumina hollow cathode lamp HCL e The second version is designed to operate with a single PerkinElmer Lumina hollow cathode lamp HCL or an electrodeless discharge lamp EDL The second version comes with a background corrector deuterium lamp D2 e The third version includes a lamp turret mount and is designed to operate with up to four PerkinElmer Lumina hollow cathode lamps HCLs or with two electrodeless discharge lamps EDLs and two PerkinElmer Lumina hollow cathode lamps HCLs The third version comes with a background corrector deuterium lamp D2 Lamp compartment The lamp compartment is located behind the door on the right hand side at the front of the spectrometer The lamp turret mount version shows the assigned lamp positions numbered 1 through 4 tagat Figure 6 10 Lamp compartment of turret version 6 21 Operation of the Instrument Installing and connecting HCLs You can use both single element and multi element hollow cathode lamps e a D Figure 6 11 Installing a hollow cathode lamp 1 Open the lamp door 2 Sli
156. like to touch the active areas of the touch screen Do not use sharp pointed objects A light short touch is all that is needed You do not need to press forcefully on an active area Note that when you touch an active area various processes may be started in the spectrometer Some of these processes take several seconds Be patient and wait for the process to complete before touching another active area on the touch screen 6 19 Operation of the Instrument User interface components The user interface components on the touch screen are described below Pages The main displays on the touch screen are termed pages You use the pages to set up your spectrometer and to perform analyses The pages contain e Entry fields which allow you to make entries via a dialog e Buttons that you touch to start or stop actions or to display a dialog e Option Buttons that you use to select an option from a list and e Check Boxes that you use to switch functions on or off Dialogs When you touch an entry field or certain buttons a dialog is displayed on the touch screen e When you touch a numerical entry field a Numerical Entry dialog containing a numerical keyboard is displayed this allows you to make numerical entry e When you touch a parameter entry field a Parameter Entry dialog is displayed you can choose among a number of options e When you touch a text entry field a Text Entry dialog containing an alphanumerical keyboard is disp
157. linder Blue nitrous oxide hose from spectometer Figure 5 7 Nitrous oxide supply connections 1 Connect the blue nitrous oxide hose coming from the back of the spectrometer to the nitrous oxide regulator 2 Tighten the connection using the double wrench technique Hold the fitting on the regulator with one wrench and tighten the compression nut on the gas hose with the other wrench NOTE Ifyou intend to perform analyses using only the air acetylene flame i e you do not intend to analyze elements that require a nitrous oxide acetylene flame you will not require a supply of nitrous oxide When shipped from the manufacturing site the blue nitrous oxide hose is fitted with a plug Leave this plug in the free end of the hose when it is not connected to a supply of nitrous oxide 5 17 Installation Connecting to the acetylene supply Warning Flammable Gas Fire and Explosion Hazard Acetylene is a flammable gas The seepage of acetylene from any gas connection constitutes a serious fire hazard Make sure that all gas connections are gas tight Check the gas connections and gas hoses regularly for leaks using a suitable leak testing fluid WARNING Acetylene regulator Flash arrestor a Acetylene cylinder Red acetylene hose from spectrometer A 1 Connect the red acetylene hose coming from the back of the spectrometer to the acetylene regulator Figure 5 8 Acetylene supply connections
158. local PerkinElmer office can supply you with the addresses of suitable suppliers In many countries electrical codes do not permit PerkinElmer service engineers to install the blower and vent assembly Blower and vent kit The blower and vent kit P N 0303 0406 available from PerkinElmer contains a rotary blower with associated hardware a hood to be located above the instrument an adapter to connect the blower and hood to suitable metal ducting and installation instructions The blower requires a line voltage of 120 V or 230 V The adapter and hood are made of stainless steel The metal ducting required to connect the hood to the blower and for the exhaust from the blower is not included in the kit 11 cm I D 4 3 in 30 cm gt 12 in 45 a ee 6 in Figure 3 4 Dimensions of a typical exhaust hoodGas Supply Requirements The permanent installation of gas supplies is the responsibility of the user and should conform to local safety and building regulations PerkinElmer recommends that cylinders be stored outside the laboratory and that gases be piped to the spectrometer system in approved gas lines e The user must provide the gas supplies regulators connectors and valves An air compressor is recommended for air A double stage or heated regulator is recommended for nitrous oxide Either the gas supplier or PerkinElmer can provide the correct regulators and valves e You must be able to reach the on off valves easil
159. longed operation of the nitrous oxide acetylene flame may cause deposits of pyrolytic carbon to build up along the burner slot WARNING WARNING CAUTION Unstable acetylides which are likely to explode when dry may be formed when aspirating high concentrations of silver copper or mercury salts into an acetylene flame Warning Hydrochloric and Nitric Acids Risk of Burns Hydrochloric HCI and nitric HNO3 acids are corrosive and can cause severe burns If high concentrations of Cu Ag or Hg have been aspirated into an acetylene flame clean the burner chamber immediately after use by following the procedures in this section called Cleaning the Burner After Aspirating Cu Ag or Hg sample 9 17 Maintenance Flashbacks A flashback is an explosion of the premixed gases in the burner chamber The safety interlocks normally prevent conditions that could cause a flashback but if a flashback should ever occur e Check that the burner head slot is clean e Check that the burner head is seated correctly e Check the flow spoiler or impact bead for damage and replace any damaged parts e Make sure that you are using compressed air and not oxygen enriched air Carefully check and tighten all connections to and seals on the burner unit and check the gas flow settings before you attempt to ignite the flame Seepage of fuel and oxidant from the burner chamber may cause a flashback 9 18 NOTE AAnalyst 200 Us
160. lts and in extreme cases may cause a potential safety hazard In general if cylinder air is to be used it is important to specify compressed air rather than breathing air and that the oxygen content is less than 20 Warning Flashback Hazard PerkinElmer burner systems are designed for use with compressed air The use of oxygen can cause an explosion in the burner system and oxygen enriched air WARNING can cause a flashback of the flame Never use oxygen or oxygen enriched air with PerkinElmer burner systems Use only compressed air Nitrous oxide supply requirements Warning Nitrous oxide is a strong oxidant and an asphyxiant WARNING Nitrous oxide is an asphyxiant it can be considered a potential hazard whenever it is stored or used in a confined space Spontaneous combustion may occur if nitrous oxide comes into contact with grease oil or other organic material e Store nitrous oxide cylinders in a well ventilated area outside the laboratory Do not store nitrous oxide cylinders in close proximity to flammable gases e g acetylene Make sure tubing and fittings carrying nitrous oxide are free of grease oil or other organic material 3 17 Preparing Your Lab Cylinder information The nitrous oxide supply should be at least 99 pure Cylinders of nitrous oxide are available from local suppliers Nitrous oxide is supplied in the liquid state initially at a pressure of about 5000 kPa 725 psig A siz
161. lyses Results of each analysis are displayed on the Results Window When the system finishes the analysis of each solution the most recent results are added to the bottom of the Results Window Standard 1 0 092 0 0006 0 6 Standard 2 0 178 0 0007 0 4 Standard 3 0 272 0 0009 0 3 Analyze All Sample Locations 5 to f M Sample Info Calibrate Recalibration Frequency b Display Calibration Analyze Samples Autosampler Tray E 200 Printer On Off Screen 7 15 Analyze Page Autosampler Results Window on the Analyze Page Autosampler This window displays the standards and sample measurements Sample This displays specific information about each solution analyzed For example blank standard 1 standard 2 sample 1 sample 2 etc Mean This displays the mean concentration in sample units or absorbance SD This displays the standard deviation RSD This displays the relative standard deviation also 7 25 Touch Screens Replicates referred to as the coefficient of variation This displays the replicate information for each replicate analyzed Buttons on Analyze Samples page Analyze All Calibrate Analyze Samples Display Calibration Printer On Off By touching this button the system will start an automated analysis of the blank standards and samples A green light appears on the button when selected Touch this button to start the calibration sequence The system uses the blank and standard
162. m Works The basic instrument includes a burner system for flame sampling operation A system block diagram is shown in the next figure As previously mentioned the heat produced by the burner converts the sample into free atoms that can absorb the light from the source lamp for the element s A sample solution is aspirated through the nebulizer and sprayed as a fine aerosol mist into the burner chamber Here the sample mist is thoroughly mixed with the fuel and either air or nitrous oxide gases Fuel gas enters the chamber through the fuel inlet hose while the oxidant enters through the nebulizer side arm and the AUX oxidant inlet To prevent incomplete sample atomization a plastic flow spoiler is placed inside the chamber directly in front of the nebulizer The nebulizer utilizes a ceramic one piece impact bead structure which improves nebulization efficiency Larger sample droplets not carried around the flow spoiler by the gas flow are forced by the spoiler to the bottom of the chamber This in turn allows only the finer sample droplets to be carried into the chamber The larger droplets are removed through the drain Once the sample mist is thoroughly mixed in the chamber it is carried to the burner head Once there the flame causes dislocation and atomization The gas control system monitors and controls fuel and oxidant flows Burner operation including flame ignition flame shutoff and gas flow settings is controlled through the
163. me tab to display the Flame page Aspirate the blank solution and when the signal is steady touch the Auto Zero Graph button Aspirate the standard solution Turn the nebulizer regulator slowly counter clockwise until bubbles start to appear from the end of the sample tube in the standard solution Then turn the nebulizer regulator 1 to 1 2 turns clockwise Slowly continue to turn the regulator clockwise while watching the continuous graphics display The absorbance reading will increase to a maximum before starting to decrease Adjust the regulator to give the maximum reading 6 38 AAnalyst 200 User s Guide Optimizing the Burner System Summary of the optimization procedure 1 Perform the preliminary steps 2 Prepare the required solutions 3 Install a lamp for the analyte element 4 Start up the spectrometer 5 Set up the burner system 6 Perform the safety checks Ignite the flame 7 Optimize the burner position Optimize the nebulizer 8 Optimize the gas flow rates Preliminary steps Before you optimize the burner system for your particular analyses perform the following preliminary steps 1 Set up the burner system and make sure that the correct burner head is installed 2 Check that the burner height has been correctly set 3 Make sure that you have preadjusted the nebulizer Preparing the solutions The blank and standard solutions should be the same as those you will use when analyzing samples
164. mization This section contains a summary of the hazards associated with the flame atomization technique For more detailed information see the remaining sections in this safety chapter High temperatures The flame can generate temperatures of up to 2800 C To avoid serious burns never touch the burner head until it has cooled to room temperature WARNING Toxic products e Toxic combustion products can be generated by the system depending on the type of analyses being performed You must provide an efficient exhaust venting system to remove toxic products generated during instrument operation e Combustion products may vary with the analysis of each sample Acetylene less than 1 liter is released during the bleeding of the gas box prior to shutdown An exhaust venting system is always required to remove those gases which are generated during the normal operation of the instrument e The materials in sample and reagent containers and material that you collect in waste containers may include small amounts of toxic substances that were used in the analyses You may have to dispose of these as hazardous waste UV radiation You should be aware of the health hazard presented by UV radiation Always wear UV absorbing eye protection when viewing e The flame especially the nitrous oxide acetylene flame e Hollow cathode or electrodeless discharge lamps e The deuterium background correction lamp e Keep the atomizer compartmen
165. n damage your eyes e Keep the door closed when the flame is burning unless you need to adjust the burner as described in the user documentation e Always wear the UV absorbing safety glasses when looking at the flame WARNING Warning Flashback While the flame is on DO NOT push the lever that is located on the burner mount assembly NOTE In an emergency switch off the spectrometer using the operational on off switch behind the lamp door or the emergency flame off switch on the front of the instrument The flame is automatically extinguished and the gases shut down in a safe sequence See Chapter 8 for the procedure to follow after an emergency shutdown To ignite the flame 1 door Start up the spectrometer system The power switch is on the E Box located behind the lamp Adjust the gas supply regulator pressure to the recommended values Perform the safety checks Touch the Flame tab to display the Flame page Touch the Oxidant Tab to display the Flame Type dialog Touch the button for the required flame type Air Acetylene or Nitrous Oxide Acetylene and then touch OK 6 35 Operation of the Instrument 7 Ignite the flame Touch the On side of the Flame On Off switch The indicator in the switch lights up The correct procedure to extinguish the flame is described in this chapter If the system is set up correctly the flame is ignited using default values for the gas flows If you selected nitrou
166. n from the sample information file Blank 0 082 0 0001 0 2 Standard 1 0 350 0 0017 0 5 Standard 2 0 765 0 0041 0 5 Analyze Blank Printer On Off Analyze Standard Standard 1 10 000 mg L Display Calibration Analyze Sample fi ID Sample 001 Dilution 1 000 Parameters Screen 7 12 Analyze Samples Page Manual Data Display Flame Technique 7 20 AAnalyst 200 User s Guide Analyze Blank Printer On Off Analyze Standard Display Calibration Analyze Sample 1 ID Sample 001 Dilution 1 000 Screen 7 13 Analyze Samples Page Manual Data Display MHS Technique Results Window on the Sample Page This window displays the standards and sample measurements Sample This displays specific sample identifier about each solution analyzed For example blank standard 1 standard 2 sample 1 sample 2 etc Mean This displays the mean concentration in sample units or absorbance SD This displays the standard deviation RSD This displays the relative standard deviation also referred to as the coefficient of variation Replicates This displays the replicate information for each replicate analyzed in concentration or absorbance 7 21 Touch Screens Buttons on Analyze Samples page Analyze Blank Analyze Standard Analyze Sample Display Calibration Printer On Off To analyze the blank defined in the method touch this button A green light appears on this button when selected
167. name given to identify the stand alone computer To locate the computer name do the following procedure on the stand alone PC e Point to the My Computer icon and right click the mouse once e A shortcut menu appears and selects Properties Open Browse With Paint Shop Pro 7 Explore Search Manage Map Network Drive Disconnect Network Drive Create Shortcut Rename Properties Screen 7 20 Shortcut Menu e System Properties dialog appear and select the Network Identification tab 7 33 Touch Screens System Properties Screen 7 21 System Properties 7 Share Name A name of a drive or folder on the directory that allows other users permission to access it If you do not already have an existing shared drive or folder and need to create a shared drive or folder follow the procedure below e Open Windows Explorer and right click on the desired drive or folder to make it sharable e From the shortcut menu choose Sharing 7 34 AAnalyst 200 User s Guide Se ed Name a OLATA S e Jaa Explore Local Disk C Aa Open AD Browse With Paint Shop Pro 7 4A200 Result Data Auc Search File Folder BDE d Sharing Modified 6 28 2002 3 36 PM BO 6S Add to Zip _ BAC i Attributes normal rail tF Add to AAZ00 Result Data zip t Zip and E Mail 44200 Result Data zip ice Cat Scan for Viruses Se Neare coore Dat Send To gt dat _ das ou Cap
168. nces and warnings NOTE A note indicates additional significant information that is provided with some procedures We use the term CAUTION to inform you about situations that could result in serious damage to the instrument or other CAUTION equipment Details about these circumstances are in a box like this one We use the term WARNING to inform you about situations that could result in personal injury to yourself or other persons Details about these circumstances are in a box like this one WARNING Introduction Warning Labels on the Instrument Caution hot surface Caution risk of electric shock Warning refer to accompanying documents Figure A Label located on the front of the AAnalyst 200 oO A E 8g a s ea os oo Cc momo m y o0 I AAnalyst 200 User s Guide WARNING Hot Lamp WARNING To avoid electrical shock disconnect power cord before servicing WARNING UV Light Source Wear protective glasses when working with this cover removed Nebulizer clamp must be lowered and locked over the nebulizer flange Never use oxygen Read instructions before lighting burner Drain trap must be filled WARNING Hot surfaces Emergency flame off switch 1 7 Introduction Figure B Label located on the right side of the AAnalyst 200 AN CAUTION do not restrict air intake or exhaust AAnalyst 200 User s Guide Figure C Labels lo
169. nd 3 respectively in this example Data Display If you selected Manual Data Display for Sample Handling on Spectrometer subpage continue as described in this section Enter parameters on Lamp page 1 If not already done install and align the required lamp For more information see Chapter 6 Operation of the Instrument 2 Enter lamp parameters For more information on how to enter analytical parameters refer to Chapter 7 Touch Screen On Flame page 1 Install burner head see Chapter 6 Operation of the Instrument 2 Adjust the burner height see Chapter 6 Operation of the Instrument 3 Adjust fuel oxidant flows 4 Check interlocks see Chapter 7 Touch Screen 5 Ignite flame see Chapter 6 Operation of the Instrument 6 Adjust the nebulizer see Chapter 9 Maintenance 7 Optimize the burner system see Chapter 6 Operation of the Instrument AAnalyst 200 User s Guide On Parameters page Spectrometer subpage 1 2 Enter 1 second for the Integration Time Enter 3 for the number of Replicates Enter 5 seconds for the Read Delay Enter the required Print parameters Select Manual Data Display for Sample Handling Spectrometer A recta Integration Time sec Replicates fetatn Read Delay sec Print M Method M Replicates Sample Handling Manual Data Display Manual Continuous Graphics Display O Autosampler Parameters rN Analyze Screen 8 1 Parameters page Spectromet
170. nd pin on a three prong line cord WARNING The line cord should have the electrical rating and plug appropriate for your location See the figure below for the correct cord 1 Select the proper line cord for your location 2 Insure that the power switch is off and insert one side of the line cord plug into the instrument and the other side into the AC supply North America ae oo Standard NEMA 5 15 india 0998 8986 pee T Europe British Standard CEE 7 BS 1363 Schuko United Kingdom 0999 1415 0999 1414 7 Europe Australia gt Switzerland ETSA S 86 0999 1413 0999 1417 Europe Israel Italy 2 2 z 0999 1422 0999 1424 Denmark A Japan 0999 1416 0999 1425 Figure 4 11 The AC line cord selections for the A Analyst instrument 4 20 AAnalyst 200 User s Guide Mercury Hydride Determination System MHS 15 Mercury Hydride Systems are proven accessories for high sensitivity determinations of mercury and metallic hydride forming elements including As Se Sb Te Bi and Sn by atomic absorption spectroscopy The basic components of a mercury hydride system are the reaction vessel and sampling cell The sample solution reacts with a reducing agent in the reaction vessel A spontaneous reaction occurs to form the gaseous hydride or to reduce mercury to its elemental form The gaseous products are carried to the sample cell a quartz cell placed in the light path of the spectrometer The quartz cell is
171. nebulizer side arm Slide the nut on the end of the hose hanging free on the burner base The hose has white tape on it printed with the word NEB Slide the NEB oxidant tubing onto the ridges on the nebulizer side arm Using the Apiezon grease lightly lubricate the OUTSIDE of the tubing where the nut will screw onto the nebulizer ridges Finally slide the plastic nut up the black tubing and gently thread it over the ridges on the side arm Tighten the plastic nut just finger tight The nebulizer is now assembled in place and secure Operation of the Instrument Checking that the Burner End Cap is Secure The burner end cap is assembled to the burner chamber at the factory It is always a good idea to confirm that the screws are tight To do so hand tighten in an alternating pattern the four knurled screws holding the burner end cap to the burner chamber Tightening them in an alternating pattern diagonally opposite nuts will allow the o ring to form a good seal See the figure below for the location of the four knurled screws Tighten them only hand tight YK Burner Chamber ae Burner End Cap Knurled Screws typical 4 places Figure 6 3 Checking that the burner end cap is secure 6 8 AAnalyst 200 User s Guide Connecting and Securing the Gas Hoses to the Burner There are three gas hoses that are connected to the end cap on the burner assembly the nebulizer oxidant hose the auxiliary oxidant hose and th
172. ner lining of the drain tube does not get damaged 6 Use a flat blade screwdriver to tighten the hose clamp 7 Plug the white drain interlock connector into the drain interlock plug on the burner assembly Drain Hose Clamp Drain Interlock Connector Screen 5 7 Drain hose and drain interlock Further procedures for setting up the burner system are described in Chapter 6 Operation of the Instrument 5 20 AAnalyst 200 User s Guide Installing the Burner Door The burner door is packed separately for shipping Refer to the figure below when installing the door Burner Door Figure 5 10 Installing the atomizer compartment door 1 Hold the door in place next to the burner compartment 2 Tilt the top of the door away from the upper door pin while you push the lower pin up into the hole in the door mount 3 Drop the top pin down into the upper hole in the door mount while holding the bottom pin in place Swing the door while letting it drop down and lock into place on the hinges 4 Close the door This completes the procedure for installing the burner door 5 21 Installation Installing the Sample Tray The sample tray is packed separately for shipping Figure 5 11 Sample tray 1 Hold the tray with both hand
173. ners These elbows should turn at a centerline radius of 150mm with a maximum bend angle of 45 degrees to reduce friction losses and the number of elbows should be minimized You must provide an efficient exhaust venting system to remove heat toxic combustion fumes and vapors that can be generated by atomic spectroscopy instruments We strongly recommend that you do not place the spectrometer in a chemical hood 3 12 AAnalyst 200 User s Guide Additional recommendations on the venting system include the following items Make sure the duct casing is installed using fireproof construction Route ducts away from sprinkler heads The duct casing and venting system should be made of materials suitable for temperatures greater than 70 C 158 F They should be installed to meet local building code requirements The exhaust hood opening should be about 170 mm 6 7 inches above the top of the burner shield Locate the discharge outlet as close to the blower as possible All joints on the discharge side should be airtight especially if toxic vapors are being vented Equip the blower with a pilot light located near the instrument to indicate to the operator when the blower is on Equip the outlet end of the system with a back draft damper and take the necessary precautions to keep the exhaust outlet away from open windows or inlet vents In addition extend it above the roof of the building for proper dispersal of the exhaust Equ
174. nment Maintenance Spectrometer Maintenance Checklists Maintenance checklists for the spectrometer system are presented below General preventative maintenance procedures Instrument and For safety reasons and to avoid contaminating new samples you should make sure that the instrument and the work area are always absolutely clean This is especially important when you are working with toxic substances and when you are measuring trace amounts of any elements Wipe up spills immediately before they can cause further contamination or damage Before you leave the instrument standing idle for any period of time make sure that all the omponents are clean ake sure that the main exhaust ventilation system functions correctly Always Switch it on when you are using the instrument end windows Airfiters R eplace filter yearly or more often in a dusty environment AAnalyst 200 User s Guide Burner Maintenance Checklist Maintenance checklists for the burner system are presented below Burner system maintenance checklist If you analyze samples that have dirty matrices such as blood sugar or oil you will probably have to lean the components more often than if you were analyzing clean samples such as drinking water urner system Always rinse the burner system correctly before extinguishing the flame If you are analyzing samples with high solids content Clean the burner chamber at least once daily If you are us
175. nment You should readjust the burner any time the burner is cleaned or the burner head is replaced Installing AAnalyst Nebulizer Warning Flammable Gases Fire and Explosion Hazard The use of the wrong type of nebulizer for your burner system may result in a seepage of fuel gas which is a serious fire hazard Use only the nebulizers specified for the burner system Install the AAnalyst nebulizer using the following procedure 1 Before you install the nebulizer verify that the o rings are in good condition If an o ring appears damaged replace it 2 Holding the nebulizer with one hand remove the gas supply connector nut on the nebulizer side arm and place it over the end of the NEB oxidant tubing 3 While holding the nebulizer firmly gradually and carefully slide the NEB gas supply tubing over the barbs on the nebulizer side arm NOTE Carefully tilt the tubing up and down and rotate it while sliding it over the barbs 9 30 AAnalyst 200 User s Guide 4 Screw the connector nut onto the nebulizer side arm Tighten the connector nut so that the side arm threads are covered by the nut CAUTION Excessive tightening could result in damage to the nebulizer when you remove the nut 5 Apply a small amount of Apiezon grease onto the o rings P N 0990 2015 The nebulizer will then slide easily into the end cap when you perform steps 5 and 6 below 6 Lift the end cap spring clamp and insert the nebulizer in
176. nt in small or confined areas e Do not store cylinders near elevators gangways or in locations where heavy moving objects may strike or fall against them 2 15 Safety Practices Use and store cylinders away from exits and exit routes Locate cylinders away from heat sources including heat lamps Compressed gas cylinders should not be subjected to temperatures above 52 C 126 F Do not allow ignition sources in the storage area and keep cylinders away from readily ignitable substances such as gasoline or waste or combustibles in bulk including oil Store cylinders standing upright fastened securely to an immovable bulkhead or permanent wall When storing cylinders outdoors they should be stored above ground on a suitable floor and protected against temperature extremes including the direct rays of the sun Mark gas cylinders clearly to identify the contents and status full empty etc Do not attempt to refill gas cylinders Arrange gas hoses where they will not be damaged or stepped on and where things will not be dropped on them Perform periodic gas leak tests by applying a soap solution to all joints and seals Handling Cylinders Review the following precautions to ensure the safe use and handling of gas cylinders 2 16 If it becomes necessary to move cylinders do so with a suitable hand truck after insuring that the container cap is secured and the cylinder is properly fastened to the hand truck Us
177. o the geographical display and used in the calculation of the Peak Height when the Peak Height measurement mode is selected Automatic sets the scale based on the highest point on the plot being displayed Fixed absorbance is manually setting peak scales AAnalyst 200 User s Guide Calibration subpage 1 Touch the Calibration tab to display this subpage 2 You select the required calibration equation units and enter the concentrations of the standards calibration solutions on this page A Be mm A n A n D T I Be N E D T K M L D D D Screen 7 11 Calibration Subpage Items on this page Spectrometer Calibration Equation Units Figures After Decimal Touch entry field that displays the selected calibration equation To change the calibration equation touch this field to display the Calibration Equation dialog Select the required calibration equation and then touch OK Touch entry field that displays the selected units of concentration To change the units of concentration touch this field to display the Units dialog Select the required units and then touch OK Number of decimal places used for inputting standard concentrations and reporting calculated concentrations 7 17 Touch Screens Standard Concentrations 1 8 Reslope Touch entry fields that display the selected concentrations of up to 8 standards calibration solutions To enter the concentration of a
178. observing the continuous graphics display Continue to make adjustments until you find the flow rates that give maximum absorbance reading After making a small change in the flow rate wait a few seconds to allow the flame to stabilize before making further changes 6 42 AAnalyst 200 User s Guide Rinsing the Burner System Before you extinguish the flame or begin maintenance or disassembly procedures you must rinse the burner system After you extinguish the flame allow the burner head to cool To rinse the system The procedure for rinsing the burner system depends on the type of samples that you have analyzed Recommendations e Ifthe sample solutions contained organic solvents use a multi rinse procedure to remove all traces of the solvents from the system e If the sample solutions contained toxic substances you must rinse all traces of these substances out of the system e Ifthe sample solutions contained high concentrations of copper silver or mercury salts which can form unstable acetylides you must rinse all traces of these substances out of the system Procedures If you used only aqueous solutions during the analyses e Aspirate deionized water for 5 minutes If you used organic solvents during the analyses e Aspirate for 5 minutes an organic solvent that is miscible with the samples that have just been aspirated e Aspirate for 5 minutes methanol or another solvent that is miscible both with water
179. ock the fan operating on the right side of the instrument e Make sure that there is sufficient room for you to work comfortably with the instrument and that you can reach the connections at the rear of the instruments and the electricity and gas supply points Laboratory Space Requirements The illustrations on the following pages show the dimensions of the spectrometer and the space that you require to accommodate the spectrometer and ancillary equipment Instrument Dimensions AAnalyst 200 is 700 mm wide 27 6 in 760 mm deep 29 9 in 650 mm 25 5 in high The instrument weighs 49 kg 108 pounds The main power cable length is 2 m 6 ft To provide access for servicing and space for ventilation allow at least 25 4 cm 10 in of space between the instrument and the laboratory walls Preparing Your Lab 650 mm 910 mm Figure 3 1 Outside dimensions of instrument 3 8 AAnalyst 200 User s Guide Bench Requirement The benchtop or area in which the AAnalyst 200 instrument is to be installed should be large enough to accommodate the instrument and any accessories you ll be using The instrument itself weighs 49 kg 108 Ib If you are considering the use of other accessories the bench you choose to use should be able to sustain as much as 136 kg 300 Ibs Location Typically the system is installed on a laboratory work bench or table The table should be smooth level and free from vibration The dim
180. of water into the drain tubing 3 Carefully reconnect the drain tubing to the burner end cap Replace the drain clamp and tighten securely Installation of the burner drain is complete 9 35 NOTE Maintenance Cleaning the Nebulizer To maintain optimum nebulizer performance you must periodically clean the capillary assembly and occasionally replace the sample tube When you aspirate concentrated samples with complex matrices it is especially important to keep the burner chamber and nebulizer free of deposits It is beneficial to periodically aspirate a dilute surfactant solution such as 0 1 Triton X100 for several minutes to keep the system clean The surfactant will encourage constant drainage which is essential for optimum burner system performance If you suspect that the nebulizer is causing low absorbance readings or poor sensitivity e g cannot obtain expected characteristic concentration before cleaning the nebulizer check that e The sample tube is in good condition i e no kinks is not too long and is clean With a longer sample tube the rate of sample uptake and thus the sensitivity will decrease Recommended length 20 cm e The burner head is clean e The burner is correctly optimized e Correct operating parameters are used Clearing an obstruction in the nebulizer Clean the nebulizer capillary whenever you notice degradation in absorbance values due to blockage of the capillary There are two ways
181. ommend that you connect the spectrometer computer printer and any accessories to the same phase of the line power supply and the same protective earth The line power supply must conform to local safety regulations and be checked by a qualified electrician before you connect the instrument to line power Installation Category The AAnalyst 200 is able to withstand transient overvoltage according to Installation Category II as defined in IEC 1010 1 Pollution Degree The AAnalyst 200 will operate safely in environments that contain nonconductive foreign matter up to Pollution Degree 2 in IEC 1010 1 Instrument Grounding circuit continuity is vital for safe operation of equipment Never operate equipment with grounding conductor disconnected WARNING The instrument power cord is to be connected to a circuit with a protective circuit breaker or fuse NEMA The National Electrical Manufacturer s Association CEE International Commission on Rules for the Approval of Electrical Equipment 3 20 AAnalyst 200 User s Guide Lamps These are often called primary source lamps atomic absorption source lamps spectroscopic lamps or line sources You need to provide the lamps for your particular applications Please refer to the PerkinElmer Instruments e ssentials catalog for a list of available lamps 3 21 Preparing Your Lab 3 22 System Description 4 AAnalyst 200 User s Guide Introduction The AAnalyst
182. on on the Lamp page of the touch screen Fill in the required parameters for the uncoded lamps in the Install Lamps dialog Touch the On Off check box to turn the lamps on A total of 3 lamps may be turned on a combination of 1 HCL lamp and 2 EDLs lamps Touch the Element entry field box Select the desired element from the Select Element box Touch OK and the instrument performs an automatic setup NOTE To change the wavelength or slit touch the corresponding entry field box and select the alternate wavelength or slit AY Z gt Figure 6 15 Turret version 6 32 AAnalyst 200 User s Guide Setting the Burner Height When you operate the spectrometer for the first time and every time you have disassembled the burner for cleaning you must check and set the burner height You must perform this procedure to make sure that the burner head is located just below the radiation beam 1 Make sure that the burner system is set up properly and that the correct burner head for your intended analyses is installed Install a suitable lamp Ideally you need a lamp that emits a beam of visible radiation If not already on power up the spectrometer Do Not Ignite The Flame Hold a piece of white card above the burner head at right angles to the burner slot Observe the light spot on the card Ideally the radiation beam should pass over the length of the burner head and be approximately centered over the burner slot Lig
183. osampler tray analyze samples page 7 26 l 3 Index autosampler maintenance eee ereerereereeeeees 9 50 SEEVICING neie a A 9 50 spare palts eree eei an eres 9 50 autosamplers 0 0 ee eeceseceeeceeeeeeeeeeeeeeeee 9 53 calculated intercept analyte addition 7 19 acetylides safety o eetas ieee el oie 2 7 air compressor requirements 4 3 16 COMME CUING esseere reest reises itsasi 5 15 cylinder information eee 3 17 requirements eseseeeeeeereeeeereereeresee 3 16 WANDE rass 3 17 aligning lampieri 6 29 atomizers mercury hydride determination system 4 21 autosampler connection niar e 5 24 SetU Diae een eo e reae Enia 5 25 B background Corrector s es 6 27 7 7 bleed gases button on Flame page eee 7 13 blower information 0 cece cet ceeeceteeeeeeeees 3 13 bracketing calibration 0 0 eee 7 19 buttons analyze samples page 7 22 7 26 burner ead tise Wiese Meee eh ara 4 15 ignitor description 4 16 installation wo eee 5 19 5 21 end Ca pris Avwesiriisie edie ed tact 6 8 SAS HOSES ieee aeai ania 6 9 MOUNT eean ai a et E et 6 12 Crain SYStOM anniren 6 14 TINSING 23 02 Sises e eve ie 6 43 8 30 Safety checkin t 6 26 Setting height eeeeseeseeeeee 6 33 burner alignment controls 6 34 burner assembly removal eeee 9 23 burner chamber Cleaning es ean eas 9 12 cleaning after aspirating Cu Ag or Hg 9 13 Ind
184. oubleshooting Possible Cause of Problem Flame does not Check and or Remedy Check the interlocks Refer to The interlocks may not be satisfied ignite 10 8 for one or more of the possible reasons listed below Fuel or oxidant may not be on or at the proper pressures The proper burner head may not be installed or fully seated The 5 cm N O burner head must be used for all nitrous oxide acetylene analyses N20 C2H2 The drain interlock may not be connected The level of liquid in the drain vessel may be too low The level of liquid in the drain vessel may be too high The fuel oxidant flow stopped after 15 seconds The nebulizer interlock may not be satisfied the possible causes listed below Check fuel and oxidant Check that the pressure is maintained during the ignition cycle Check to make sure the correct burner head is installed fully seated and secured Make sure the drain interlock connection has been made Pour about 200 300 mL of deionized water into the neck of the burner or directly into the top of the drain hose Empty the drain vessel Try igniting the flame again Check that the nebulizer is properly installed with the side arm locked in place Flame does not ignite continued Burner flashes back The flame may not ignite if the ignitor tube is not positioned directly above the burner slot Flashbacks can be caused by any of the reasons listed below
185. ouch the Analyze Samples button 8 20 AAnalyst 200 User s Guide The results are displayed and printed Standard 2 Standard 3 Standard 4 Sample 001 Analyze All Sample Locations fio to Fo v Sample Info Calibrate Recalibration Frequency Display Calibration Analyze Samples Autosampler Tray 152 Printer OvO m Screen 8 12 Analyze page 8 21 Analyzing Samples Manual Analyses Data Display MHS Technique If you have selected MHS technique from the Startup dialog continue as described in this chapter Setting Up MHS 15 Analyses 1 Read the safety information in the handbooks for your system before you operate the spectrometer Make sure that the analyzer assembly and quartz cell are correctly installed See the handbooks for your system Switch on the fume ventilation system for the work area Switch on the AA200 instrument See Chapter 6 Operation of the Instrument Select the MHS technique from the startup screen or from the tools menu startup Select or fill the required touch entry fields on the Parameters page Spectrometer subpage Spectrometer Abrenes Integration Time sec Replicates foarsten Print C Method C Replicates Measurement Peak Height Peak Area Smoothing Points fis Peak Plot Scale Automatic O Fixed abs 1 00 Parameters Tools Screen 8 13 Parameters page Spectrometer subpage Install and align the
186. pages within dialogs AAnalyst 200 User s Guide Startup Dialog The following page is the first page displayed once you start up the system You use this page to select the technique Flame or MHS and to examine the system diagnostics Touch the Details bar on the screen to get details on the Power on Diagnostics In the Details dialog all entries should be in green to indicate that all systems are OK If all the entries are green touch OK in the Startup screen Screen 7 2 Startup Dialog 7 5 Touch Screens Lamp Page You use this page to select the analyte element and the basic measurement parameters You also use this page during optimization to align the lamp with systems utilizing manual lamp adjustment Signal Atomic Absorption Set Midscale Cu Element Setup Instrument Wavelength nm 324 75 Slit rm 2 7 0 8 Install Lamps Screen 7 3 Lamp Setup Page AAnalyst 200 User s Guide Parameters on Lamp page Signal Element Wavelength nm Displays the current active signal Touch entry field that displays the mode of signal measurement selected for the analysis You can touch this field to display the Signal dialog In this dialog you can choose Atomic Absorption The instrument measures the total absorption including any background attenuation that is present Background Corrected AA This feature is available if deuterium background corrector is installed The instrument measure
187. parately according to the regulatory guidelines in your area The objectives of this program are to preserve protect and improve the quality of the environment protect human health and utilize natural resources prudently and rationally Specific treatment of WEEE is indispensable in order to avoid the dispersion of pollutants into the recycled material or waste stream Such treatment is the most effective means of protecting the customer s environment Requirements for waste collection reuse recycling and recovery programs vary by regulatory authority at your location Contact your local responsible body e g your laboratory manager or authorized representative for information regarding applicable disposal regulations Contact PerkinElmer at the web site listed below for information specific to PerkinElmer products Web address http las perkinelmer com OneSource Environmental directives htm Customer Care 1 800 762 4000 inside the USA 1 203 925 4602 outside the USA 0800 40 858 Brussels 800 90 66 42 Monza Products from other manufacturers may also form a part of your PerkinElmer system These other producers are directly responsible for the collection and processing of their own waste products under the terms of the WEEE Directive Please contact these producers directly before discarding any of their products Consult the PerkinElmer web site above for producer names and web addresses 2 24 AAnalyst 200
188. paring chemical solutions always work in a fume hood that is suitable for the chemicals you are using Perform sample preparation away from the instrument to minimize corrosion and contamination Clean up spills immediately using the appropriate equipment and supplies such as spill cleanup kits AAnalyst 200 User s Guide Location and Space Requirements Bench and location requirements The location you choose for the spectrometer must fulfill the criteria listed below e Place the spectrometer on a sturdy bench or trolley cart capable of sustaining the weight The work surface must be level flat clean dry and free from vibration It should be strong and stiff enough to bear the weight of the spectrometer system over a long period without warping or bending A movable table is very convenient but make sure that the wheels can be securely locked e Position the bench or trolley out of direct sunlight and away from radiators and heaters e Position the system near to the electricity and gas supply points e Position the system so that the atomizer compartment is located beneath a suitable exhaust venting system e The instrument should not be against a wall as the instrument must be accessible from the back for servicing purposes An accessible space of at least 25 4 cm 10 in should be available behind the instrument e Make sure that there is space at the rear and sides of the system for air to circulate freely Do not bl
189. performed the set up procedures in Chapters 3 4 5 and 6 in which case the instrument will be on and the flame ignited This example runs a blank 3 standards and 3 test samples We instructed the autosampler to perform a reslope after the second test sample 1 Carry out the following steps to duplicate our example 2 Prepare solutions Set up the autosampler 3 Load the autosampler 4 Enter parameters 5 Start the run Detailed procedures follow Prepare solutions In this example we used a copper lamp and solutions of copper for our determinations However you do not have to use copper For your convenience in making substitutions we have included a table of recommended concentrations for Ag Mg Mn and Pb 1 Prepare about 200 250 mL of 1 v v HNO to use as a blank solution 2 Prepare about 200 250 mL each of three standards in 1 v v HNO of the element you want to determine Suggested standard concentrations for five elements are shown in the following table 8 16 Table 8 2 Suggested Standards AAnalyst 200 User s Guide Element Standard 1 Standard 2 Standard 3 Reslope mg L mg L mg L mg L Ag 0 2 0 5 1 0 5 Cu 0 5 1 1 5 1 Mg 0 05 0 1 0 2 0 1 Mn 0 2 0 4 0 6 0 4 Pb 2 5 10 5 3 For samples 1 2 and 3 use Standards 1 2 and 3 respectively Set up the autosampler The autosampler you intend to use must be connected to the spectrometer Installation procedures are
190. ponsible bodies should check with PerkinElmer that the proposed method will not damage the equipment NOTE The responsible body has the responsibility for carrying out appropriate decontamination if hazardous material is spilt on or inside the equipment There are two documents on the PerkinElmer public website that responsible bodies can access and complete One is Decontamination of Instrumentation and Associated Sub assemblies and the other is the Certificate of Decontamination They are used to certify the decontamination process was completed before equipment can be returned to PerkinElmer and may serve as a format for similar customer documents 2 21 NOTE Safety Practices Waste Disposal Contents of waste containers The materials that you collect in waste containers may include small amounts of the substances that were analyzed and other chemicals used in the analyses If these materials are toxic corrosive or contain organics you may have to treat the collected effluent as hazardous waste Refer to your local safety regulations for proper disposal procedures The responsible body is responsible for the correct collection and disposal of waste materials This includes the necessity for a suitably sized waste container of appropriately resistant material for the collection of organic solvent waste and provision for the removal into an appropriate exhaust system of any gases or vapors which may be produced in hazardo
191. produced by some samples e _ It helps to protect the instrument from corrosive vapors that may originate from the sample s e It removes dissipated heat produced by the instrument and power supply e It will tend to reduce the effects of room drafts and the laboratory atmosphere on flame stability The use of the AAnalyst 200 without adequate ventilation to outside air may constitute a health hazard For example the combustion of halogenated hydrocarbons produces toxic vapors g D WARNING Temperatures The following temperatures have been measured with a nitrous oxide acetylene flame 310 C at the vent intake 160 C at 2 4 meters 8 feet from the vent intake 105 C at the blower intake and 50 C at the blower motor housing near the front bearing To withstand these temperatures stainless steel tubing must be used Local electrical codes do not allow PerkinElmer Service Engineers to install the blower and vent assembly Exhaust ducting Alternatively smooth stainless steel tubing should be used instead of flexible stainless steel tubing where flexibility is not required to reduce system friction loss or drag If smooth stainless steel is used there must be a way to move the vent hood out of the way for servicing A length of smooth stainless steel ducting has 20 30 less friction loss than a comparable length of flexible ducting When smooth stainless steel tubing is used elbows must be used to turn cor
192. pter Kit P N 0303 0870 Connect the lamp to the turret using the non coded lamp adapter P N N305 0196 or N305 0197 Contact the lamp manufacturer for further information Connect the lamp using an adapter cable if necessary Turn instrument on or plug into line power Connect lamp Try another lamp Set the proper current Check the lamp cable plug it in if it is not already Single lamp unit Adjust the position of the lamp Instrument with Turret the turret is self aligning It may be possible to continue using a hollow cathode lamp for a short period of time by increasing the lamp current up to the maximum value listed on the label on the lamp Otherwise it may be necessary to replace the lamp Check and or Remedy Adjust the lamp current Use the recommended value listed on the lamp label 10 11 Troubleshooting 10 12 The electrodeless discharge lamp current setting may be too low The slit width may be too small The wrong wavelength for the element may be specified Adjust the lamp current Use the recommended value listed on the lamp label Check the recommended settings for the element in the Recommended Conditions window Refer to the Recommended Conditions window for the element AAnalyst 200 User s Guide Troubleshooting Deuterium Background Corrector Problems Background correction requires the use of both the primary and the continuum source It is important th
193. r diagnostic purposes AAnalyst 200 User s Guide Sample Information Untitled T Sample Number Sample ID Dilution Factor Column Fill Column Fill 1 000 1 000 1 000 1 000 1 000 1 000 1 000 1 000 Print 1 000 ji 000 C External Keyboard m rs m Screen 7 17 Sample Information Dialog Buttons on Sample Information Dialog Sample Number The range of sample numbers being displayed 10 at a time in the table can be changed by using the scroll bar A maximum of 250 samples can be displayed Sample ID Shows the sample ID for each sample Clicking on an entry field will bring up the existing keyboard dialog where you can enter an ID for that sample Sample ID Column Click on this button to open the Sample ID Column Fill dialog to Fill button automatically fill in the ranges of sample IDs Dilution Factor This column shows the dilution factor for each sample Clicking on an entry field will bring up the existing numerical value where you can enter a dilution value for that sample A dilution value of 0 001 9999 can be entered Dilution Factor Click on this button to open the Dilution Factor Column Fill dialog Column Fill button which can be used to automatically fill in ranges of dilution factors Scroll Bar Use the scroll bar to scroll through the list of 250 samples 7 29 Touch Screens OK button New button Open button Save button Dele
194. r it is stored or used in a confined space WARNING Spontaneous combustion may occur if nitrous oxide comes into contact with grease oil or other organic materials e Store nitrous oxide cylinders in a well ventilated area outside the laboratory e Do not store nitrous oxide cylinders in close proximity to flammable gases e g acetylene e Make sure tubing and fittings carry nitrous oxide are free of grease oil and other organic material Warning Acetylene Explosion Hazard Acetylene can decompose explosively at pressure higher than 103 kPa 1 03 bar 15 psig e Always make sure that the acetylene outlet gauge pressure is below these values Acetylene can react with copper to form a readily explosive compound WARNING e Never use copper tubing or fittings for acetylene lines Make sure that all gas connections are gas tight Check the connections and gas hoses regularly for leaks using a leak testing fluid 2 14 NOTE AAnalyst 200 User s Guide Safe Handling of Gas Cylinders Gases commonly used with the AAnalyst 200 include acetylene nitrous oxide argon and nitrogen The major hazard associated with these gases is suffocation This can occur if the gas is allowed to escape in an enclosed area and displaces the oxygen in the air Contact the gas supplier for a material safety data sheet MSDS containing detailed information on the potential hazards associated with the gas Carefully use store and handle compressed gase
195. r subpage continue as described in this chapter Overview Once the system has been powered up and optimized analyzing samples is simply a matter of entering parameters then the autosampler starts aspirating solutions of a blank standards and test samples The AAnalyst 200 has the capability to use up to eight calibration standards and a choice of calibration equations An example of an aspirating sequence for linear nonlinear calibration is shown below Blank Standard 1 Standard 2 4 Standard 8 Sample 1 Sample 2 4 Sample 20 Recalibrate Sample 21 Sample 22 etc For nonlinear or linear calibration you can instruct the autosampler to aspirate a reslope standard at any point after the first sample is run This chapter contains an example of how to run Flame AA analyses with an autosampler using linear nonlinear and analyte additions techniques The examples take you step by step through the required procedures 8 15 Analyzing Samples Analyzing Samples Using Linear Calibration The following example describes how to run samples using the linear calibration technique It should be noted that the same steps are carried out when using the nonlinear calibration technique The only difference is in setting up the calibration type Instead of selecting nonlinear for the calibration type you select nonlinear EXAMPLE Determining copper using linear calibration The procedures in this example assume that you have
196. ration continued Cannot get suggested detection limits 10 6 Possible Cause of Problem The nebulizer may be clogged Lamp current may be improperly set too high Too much liquid may be building up in the burner chamber The burner head may be skewed in the light path The burner position may be incorrect The instrument may have been autozeroed while a sample was being aspirated Characteristic concentration may not be within 20 of the standard conditions value Integration time may be insufficient Check and or Remedy Clean the nebulizer using the procedure given in this User s Guide Reset lamp current Check for proper drainage Position the burner head so that it is parallel to the light beam Adjust the horizontal vertical and rotational position using the information in this User s Guide Autozero the instrument while aspirating a blank Check to make sure the characteristic concentration is within 20 of the specified value If it is not refer to the information on characteristic concentration above before performing the following checks Try longer integration time Data noisy with flame off Data noisy when aspirating blank Background correction not producing expected results Possible Cause of Problem Incorrect wavelength may have been selected Lamp current may be too low or the lamp may be at the end of its useful life Lamp may be unstable or
197. re are o rings in the neck of the burner chamber and in the burner end cap You must check the condition of these o rings at regular intervals and replace them if they are damaged or show signs of deterioration Warning Flammable Gases Fire and Explosion Hazard fi N WARNING If the o rings in the burner system are damaged or have deteriorated they may no longer form a proper seal This may result in a gas leak which is a serious fire hazard Check the condition of the o rings regularly and replace them if they are damaged or show signs of deterioration 1 Take the burner system apart 2 O ring located in the neck of the burner chamber Carefully lever the o ring out of the neck of the burner chamber using a plastic pipette tip or the like NOTE Never use sharp or pointed tools to remove the o ring Examine the o ring If it is damaged replace it 1 Place the o ring back into the neck of the burner chamber and press it down with your finger 2 O ring located in the burner end cap Very carefully roll out the o ring with your finger 3 Examine the o ring If it is damaged replace it 4 Gently place the o ring back into the end cap and press it into place with your finger 5 Reassemble the burner system Nebulizer O Rings There are 3 o rings on the nebulizer Always carefully check the condition of these o rings whenever you take the nebulizer apart 9 45 Maintenance E Box All electronics are locate
198. re of the health hazard presented by UV radiation e When the instrument is on do not remove any covers unless specifically instructed to do so in the guide or you may be exposed to potentially hazardous UV radiation e Always wear UV absorbing eye protection when viewing e The flame especially the nitrous oxide acetylene flame e Hollow cathode or electrodeless discharge lamps e The deuterium background correction lamp 2 11 Safety Practices High Temperatures Burner system The flame can generate temperatures of up to 2800 C To avoid serious burns never touch the burner head until it has cooled to room temperature Quartz tube atomizer The quartz tube atomizer QTA used for the hydride generation technique option can reach temperatures of up to 1000 C e To avoid serious burns never touch any part of the QTA mount flame heated systems or the QTA until they have cooled to room temperature 2 12 AAnalyst 200 User s Guide Electrical Safety The instrument has been designed to protect the operator from potential electrical hazards This section describes some recommended electrical safety practices Lethal voltages are present at certain areas within the instrument Internal maintenance of the instrument should only be performed by a PerkinElmer service engineer or similarly authorized and trained person When the N WARNING instrument is connected to line power opening the instrument covers is l
199. re than 0 05 g of analyte material 2 22 NOTE AAnalyst 200 User s Guide Electromagnetic Compatibility EMC Regulatory Information United States FCC This equipment has been tested and found to comply with the limits for a Class A digital device pursuant to part 15 of the FCC Rules These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment This equipment generates uses and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause harmful interference to radio communications Operation of this equipment in a residential area is likely to cause harmful interference in which user will be required to correct the interference at his own expense Changes or modifications not expressly approved by PerkinElmer could void the user s authority to operate this product Europe All information concerning EMC standards is in the Declaration of Conformity and these standards may change as the European Union adds new requirements 2 23 Safety Practices WEEE Instructions for PerkinElmer Products or A label with a crossed out wheeled bin symbol and a rectangular bar indicates that the product is covered by the Waste Electrical and Electronic Equipment WEEE Directive and is not to be disposed of as unsorted municipal waste Any products marked with this symbol must be collected se
200. reen 8 3 Analyze page Analyzing Samples Screen 8 4 Display Calibration screen 8 10 AAnalyst 200 User s Guide Continuous Display If you selected Manual Continuous Graphic Display for Sample Handling on Spectrometer subpage continue as described in this section Enter parameters on Lamp page 1 Ifnot already done install and align the required lamp For more information see Chapter 6 Operation of the Instrument 2 Enter lamp parameters For more information on how to enter analytical parameters refer to Chapter 7 Touch Screen On Flame page 1 Install burner head see Chapter 6 Operation of the Instrument 2 Adjust the burner height see Chapter 6 Operation of the Instrument 3 Adjust fuel oxidant flows 4 Check interlocks see chapter 7 Touch Screen 5 Ignite flame see Chapter 6 Operation of the Instrument 6 Adjust the nebulizer see Chapter 9 Maintenance 7 Optimize the burner system see Chapter 6 Operation of the Instrument On Parameter page Spectrometer subpage 1 Enter 1 second for the Integration NOTE The default for Replicate in continuous mode is 1 2 3 Enter 0 seconds for the Read Delay The default value is zero Enter the required Print parameters Select the information you would like to have printed together with the analytical results Select Manual Continuous Graphic Display for Sample Handling 8 11 Analyzing Samples N T K I D N I IN N
201. rmance and damage the lamp 1 Once you have removed the deuterium lamp assembly from the instrument place the assembly on the lab bench 2 Unscrew the bracket thumbscrew 3 Slide the bracket and bulb to remove it from the assembly NOTE Remember when handling the new lamp do not handle the glass only the metal lamp bracket 4 Replace the assembly with a new bracket bulb set by sliding under the two plastic tabs 5 Rescrew the bracket assembly 6 You have completed replacing the deuterium lamp 9 53 Maintenance Reassembling the Deuterium Lamp Assembly Next you will put the deuterium lamp assembly back into the instrument 1 Plug in the lamp cable 2 Gently set the deuterium lamp plate assembly back into place in the instrument 3 Reinstall the 4 Phillips head screws into the plate and tighten down the cover Reassembly is complete Next you may have to align the deuterium lamp Aligning Deuterium Lamp Alignment Screws Figure 9 19 Location of the alignment screws of the deuterium lamp 1 Set up the standard conditions for copper including slit 2 Goto BG mode background corrected AA and after warming the lamp for several minutes 3 Adjust the alignment screws Figure 9 19 to obtain maximum energy counts 4 Place a white card in the center of the sample compartment and note the positions of the beams from the deuterium lamp and the Hollow Cathode Lamp To complete the peaking procedure
202. rn the two alignment controls alternately and in small increments while watching the AA bar graph and the numerical energy display Align the lamp to obtain maximum energy oded single element Intensitron lamp Start up the spectrometer but do not ignite the flame Touch the Install Lamps button on the Lamp page of the touch screen The Install Lamps dialog is displayed Touch the Element entry field box on the Install Lamps dialog to display the Element dialog Select the desired element Select the proper lamp type EDL or HCL AAnalyst 200 User s Guide Touch the On Off check box If necessary change the lamp current Touch OK Touch the Element entry field box to select the desired element Touch OK Touch the Setup Instrument button on the Lamp page of the touch screen The recommended parameters for that element are automatically set up e The system automatically switches the lamp on sets up the optical path prism and grating sets and peaks the wavelength sets the slit and performs an Automatic Gain Control AGC and Automatic Intensity Control AIC Turn the two alignment controls alternately and in small increments while watching the AA bar graph and the numerical energy display Align the lamp to obtain maximum energy Uncoded multi element Lumina lamp 1 2 Follow steps 1 5 of the coded single element Lumina lamp Touch the Element entry field box on the Lamp page to display the Select Element dialog Sele
203. rner Mixin Flow Spoiler eae Impact Bead Structure Spacer End Cap Figure 6 1 Installing the nebulizer onto the burner end cap 1 Feed at least 6 8 inches 152 203 mm of capillary tubing onto the nebulizer inlet 2 Lightly lubricate the nebulizer o rings with the Apiezon grease supplied in the nebulizer kit 3 Locate the nebulizer clamp Detail A and slide it up while inserting the nebulizer into the burner end cap Be sure to orient the nebulizer side arm so that it will lie in the slot provided A gentle twisting and pushing motion might be necessary to fully seat the nebulizer in the burner end cap AAnalyst 200 User s Guide Lower the nebulizer clamp until it presses against the barrel and flange of the nebulizer shaded area Ensure that the nebulizer is pushed in all the way and clamped in correctly Warning the nebulizer clamp must be lowered and locked OVER the nebulizer flange Detail B shows the clamp lowered and locked correctly over the nebulizer flange Detail A Detail B Nebulizer Clamp one WARNING see information below in raised position iy Nebulizer A range WARNING Nebulizer Clamp must be lowered and locked OVER Nebulizer Flange Never use oxygen Read instructions before lighting burner Drain trap must be filled Figure 6 2 Installing nebulizer onto the burner end Next you ll connect the nebulizer oxidant hose to the nebulizer side arm Remove the plastic nut from the
204. roubleshooting for your burner system troubleshooting information Included are suggestions to help you determine systematically whether instrument problems are due to improper analytical techniques improper selection of instrument parameters or a malfunction of the instrument Burner Spare Parts and Accessories Refer to the end of Chapter 9 Maintenance for burner system spare parts information 4 18 AAnalyst 200 User s Guide Connecting the Electrical Supply A Review of the Electrical Specifications The electrical supply voltage must be between 100 230 VAC 10 The electrical supply voltage should be free of line transients in excess of 50V peak If the supply voltage produces large AC line voltage fluctuations install a voltage regulator between the AC outlet and the instrument The spectrometer requires either a 100 120 VAC standard 15 amp grounded outlet or a 230 VAC outlet In addition the instrument consumes 300 volt amps maximum when configured for background correction The AAnalyst 200 requires a grounded AC outlet providing voltage corresponding to the voltage range marked on the instrument 100 230 VAC Do not remove or alter the ground prong on a three prong power plug WARNING 4 19 System Description Installing the AC line Cord Grounding circuit continuity is vital for safe operation of equipment Never operate equipment with grounding conductor disconnected Do not remove or alter the grou
205. roubleshooting 1 0 AAnalyst 200 User s Guide Introduction PerkinElmer spectrometers are designed for routine trouble free operation Many errors are diagnosed immediately as they occur and a message containing details of the problem appears in the Diagnostics window Often this information enables you to solve the problem quickly Some difficulties may not be so easily diagnosed and solved For this purpose troubleshooting suggestions are included to help you determine whether the difficulties are due to unsuitable analytical techniques incorrect instrument parameters or a malfunctioning of the instrument If after checking the instrument against the symptoms described below the instrument appears to be malfunctioning we strongly recommended that you contact your local PerkinElmer service representative Servicing of the instrument by someone other than a PerkinElmer trained and authorized person will render the warranty null and void Customer Service PerkinElmer LLC 710 Bridgeport Avenue Shelton CT 06484 4794 U S A Tel 1 800 762 4000 1 203 762 4000 Internet http www perkinelmer com 10 3 Troubleshooting Flame Analysis Troubleshooting Some possible problems associated with flame analyses are listed below along with probable causes and suggested remedies It is suggested that you use this checklist to diagnose possible problems before contacting service for assistance Results erroneously high Results erron
206. rvicing of the Autosamplers may only be performed by a trained PerkinElmer Service Representative Contact your local PerkinElmer representative to schedule a service call 9 56 AAnalyst 200 User s Guide MHS 15 Mercury Hydride System Maintenance Refer to the MHS 15 User s Guide 0993 5288 for maintenance details Replacing or Installing the MHS 15 Quartz Cell Holder This section describes how to install the quartz cell holder B300 0350 onto the burner head The following section describes how to then install the quartz cell the flame if lit and allow adequate time for the burner head to cool 1 Make sure the two adjusting screws in each clamp are loose Place the securing clamps of the cell holder bracket over the ends of the burner head Rear View Cell Holder Bracket in up position Adjusting Screw pee 2 each Clamp Cell Holder Securing Clamp 1 of 2 Mounting Bracket Magnetic ID Strip Burner Head Figure 9 21 Mounting the quartz cell holder onto the burner head rear view 2 Refer to the next figure and align the V in the cell holder with the slot in the burner head 9 57 Maintenance Cell Holder Bracket in Down Position Right Hand Securing Clamp Slot in umer Align V in Head Ce ap racket with Slot in Burner Head aoa Shoulder V in Screw Cell Holder Left Hand Securing Clamp Figure 9 22 Adjusting the position of the cell holder bracket 3
207. s e Inspect the burner assembly see checklist later in this chapter e Inspect the drain system e Optical Check the window surfaces in the sample compartment for fingerprints dirt lint etc Clean the windows with a tuft of cotton moistened with a dilute solution of isopropanol followed by several rinsing with deionized water e Ifthe energy of the primary source lamp is too low refer to the lamp troubleshooting information in the Troubleshooting chapter of this manual The lamp may need to be realigned or replaced if it is old e Ifthe intensity of the deuterium arc background corrector source is too low refer to the troubleshooting information in the Troubleshooting chapter of this manual The background corrector source lamp may need to be realigned or replaced e Normally the spectrometer optics will require little or no maintenance However low energy lamp readings or noisy or erratic results may indicate that the optics require cleaning or alignment This should only be done by a PerkinElmer service engineer e A service technician may clean the mirrors by careful use of a clean cotton cloth moistened with a clean solvent such as alcohol Quick drying of the surfaces is important Do not rub optical surfaces If mirror surfaces become dirty e g from exposure to laboratory vapors cleaning should be done only by a CAUTION PerkinElmer service engineer If a service engineer is not available a skilled technician may cle
208. s defined in the method To analyze samples touch this button A green light appears on the button when selected The system will analyze sample range specified in the Sample Locations entry field box To display the calibration curve window touch this button By default the print function is On and the results will print when the printer queue is full The green light indicates that it is On To turn print function Off touch Printer On Off button This will print any results in the printer queue Parameters on Analyze Samples page Autosampler Tray First Sample Location Last Sample Location Recalibration Frequency 7 26 This shows the name of the sample tray currently selected To select a different tray touch this entry field for tray dialog This shows the starting position of the sample located on the autosampler tray To change the start sample location touch this entry field for a number pad entry dialog This shows the terminating position of the sample located on the autosampler tray To change the terminating sample location touch this entry field for a number pad entry dialog The system analyzes the calibration blank and all the calibration standards or reslope if selected and defined then creates a completely new calibration curve To set the frequency touch this entry field for the number pad dialog AAnalyst 200 User s Guide Tools Dialog You can access the Tools dialog by touching
209. s in cylinders Gas cylinders can be hazardous if they are mishandled WARNING The permanent installation of gas supplies is the responsibility of the user and should conform to local safety and building codes If liquid nitrogen is used the gas cylinder must be fitted with an over pressure regulator which will vent the cylinder as necessary to prevent it from becoming a safety hazard Listed below are some general safety practices for the proper identification storage and handling of gas cylinders Consult the following references for more detailed information and additional guidelines e Compressed Gas Association USA Safe Handling of Compressed Gases in Containers pamphlet no P 1 1984 e Compressed Gas Association USA The Inert Gases Argon Nitrogen and Helium pamphlet no P 9 1992 Identification of Gas Cylinders e Legibly mark cylinders to identify their contents Use the chemical name or commercially accepted name for the gas Storing Cylinders Review the following precautions to ensure the safe use and storage of gas cylinders e Cylinders should be stored in accordance with the regulations and standards applicable to the customer s locality state and country e When cylinders are stored indoors in storage rooms the storage room should be well ventilated and dry Ensure that the ventilation is adequate to prevent the formation of dangerous accumulations of gas This is particularly importa
210. s in the position shown in front of the instrument 2 Tilt the tray mounting posts downward at a slight angle as you insert them into the slots in the front of the instrument 3 Slide the tray all the way into the front of the instrument base until it hits the stop At that point gently push the tray edge downward to secure it into place You will feel it lock into place NOTE Do not block access to the E Box located behind the right front cover Removal of the power cord from the appliance coupler will completely disconnect the AAnalyst 200 from AC power line This completes the procedure for installing the sample tray 5 22 AAnalyst 200 User s Guide Connecting to the Electrical Supply After you have completed the installation procedures described previously connect the spectrometer to the electrical supply 1 5 6 Check the line cord provided with the spectrometer to make sure that it is fitted with the correct plug for your location If the plug is not correct contact your local PerkinElmer office for advice Make sure that the On Off switch on the spectrometer s E Box behind the lamp door is in the Off position depressed Pass line cord receptacle underneath through the slot at the bottom of the lamp compartment Insert the line cord receptacle into the line power input module on the E Box Insert the line cord plug into a suitable electrical outlet Do not switch on the spectrometer yet The correct
211. s oxide as the flame type the flame is ignited with an air acetylene mixture with automatic changeover to nitrous oxide after several seconds NOTE It is recommended to warm up the burner head with air acetylene flame for 15 minutes before switching to nitrous oxide flame 10 The flame should appear uniform and stable throughout its length If it is not even after WARNING warming up you may need to clean the burner head See the Maintenance chapter in this User s Guide Manual The nitrous oxide acetylene flame may split and form a V along the burner slot when it is first ignited As the burner head warms up the V will close This may take several minutes When using nitrous oxide the flame should have a red plume Increase the oxidant flow until the red plume is 17 2 inches to 1 inches high Select an air acetylene flame If you are preadjusting the nebulizer If you have installed a different nebulizer cleaned the nebulizer or if the settings on the nebulizer have been altered since it was last used If you are using the flame to heat the quartz tube atomizer of an optional MHS 15 Mercury Hydride System 6 36 NOTE AAnalyst 200 User s Guide Preadjusting the Nebulizer In this procedure you adjust the aspiration rate solution uptake rate of the nebulizer You must preadjust the nebulizer whenever you install a nebulizer or when you have partially or totally dismantled the nebulizer for any reason such
212. s the total absorption from the analyte element and the background and then measures the signal from the background The difference between the two is the background corrected atomic absorption Flame Emission The system measures the total emission intensity using the technique of flame emission The intensity of light emitted is related to the concentration of the element in the sample Flame emission is not available in MHS technique Displays the current active element Touch entry field that displays the element to be determined analyte element If you have installed a single element coded lumina lamp the element is displayed automatically and the recommended parameters for that element are automatically set up If you have installed a multi element coded lamp you can touch this field to display the Element dialog You select the desired analyte element from the list in the dialog and the recommended parameters for that element are automatically set up If you have installed an uncoded lamp touch Install Lamps button to display the Install Lamps dialog Use this dialog to fill in the required element s and its parameters Then touch the Element entry field box to select the element Displays the current active wavelength Touch entry field that displays the wavelength of the analytical line selected to measure the absorption If more than one analytical line is available for an element you can touch this field to displ
213. sel e Then add water to the drain trap to activate the function 9 10 AAnalyst 200 User s Guide Changing the Air Filter 1 To make sure that the electrical components in the spectrometer are properly cooled the air filter must allow sufficient air into the instrument Check the filter regularly and change it if it is dirty You should not need to change the filter more than once every year if the environmental conditions are as described in the Spectrometer Maintenance Checklist of this chapter Replacement filters are available see Replacement Parts and Accessories later at the end of this chapter for the part number 2 Locate the air filter on the right side of the instrument 3 Depress the latch and lift out the plastic grid that holds the air filter in place 4 Replace the air filter and then put the grid back into place Figure 9 1 Air Filter 9 11 Maintenance Extinguishing the Flame Before you extinguish the flame or begin maintenance or disassembly procedures you must rinse the burner system After you extinguish the flame allow the burner head to cool To extinguish the flame 1 With the flame still burning aspirate the correct rinsing solutions to rinse the burner system Either aspirate the solutions manually or use the flame autosampler 2 Touch the Flame tab to display the Flame page 3 Touch the Off side of the Flame On Off switch The indicator in the switch extinguishes The system uses
214. ses where you have to shut down the system quickly and you do not have time to carry out the correct procedure you can use the procedure described below NOTE This procedure is for use in an emergency only Do not use it as a routine shutdown procedure 1 Press the Emergency Red button located on the upper left hand side of the instrument 2 When flame is extinguished shut off gases at source and bleed 3 Switch off the spectrometer at the operational on off switch on the front panel 4 Ifyou were previously running concentrated salt solutions organic solvents or solutions containing cyanide copper silver or mercury proceed as follows to shut down the system properly Wait until the instrument cools down then proceed as follows e Remove the burner head e Pour a large quantity of deionized water slowly through the neck of the burner chamber to thoroughly flush the chamber and the drain system e Check the burner head e Ifthere are deposits along the slot clean the burner head Reinstall the burner head 8 32 AAnalyst 200 User s Guide Rinsing the Burner System Before you extinguish the flame or begin maintenance or disassembly procedures you must rinse the burner system To rinse the system The procedure for rinsing the burner system depends on the type of samples that you have analyzed Recommendations e Ifthe sample solutions contained organic solvents use a multi rinse procedure to remove all tr
215. stallation AAnalyst 200 Shipping List The following parts are included in the shipment Table 5 1 Shipping List Description AAnalyst 200 Instrument Burner Door in a box Touch Screen in a box Drain Assembly including the drain vessel Installation Kit including the multimedia CD 5 8 AAnalyst 200 Spares Kit AAnalyst 200 User s Guide The following parts are included in the AAnalyst 200 Spares Kit P N B315 0021 The kit is shipped with the instrument Table 5 2 Spares Kit Part No Description QTY N315 0188 Nebulizer Kit 1 BO019 1060 Nebulizer tubing 1000mm 1 B315 0458 Nebulizer tubing 300mm for manual sampling B050 1696 Air Filter 1 0941 0063 Serial Cable 1 0990 3004 Hose Clamp 1 0998 8986 Line Cord North America 1 0999 1415 Line Cord Europe 1 0303 1573 Burner Cleaning Tool 1 N315 0188 AA 200 400 Nebulizer Kit 1 N101 0235 Quick Start CD 1 0990 9390 AA Newsletter Subscription 1 Form 0993 6643 AAnalyst 400 Safety Booklet 0943 2046 Software Utilities CD 1 0993 6550 AA Instrument Maintenance 1 Log 0993 8893 Software Spectrometer 1 Registration Card 5 9 Installation Installing the Touch Screen The touch screen is packed separately for shipping To facilitate installation of the touch screen you must temporarily remove the lamp door Figure 5 3 Removing lamp door Remove
216. standard touch the required field to display the Standard Conc dialog Enter the required concentration and then touch OK Reslope can only be used with equations linear through zero non linear through zero and linear through zero calculated intercept Touch entry field that displays the selected concentrations of the reslope solution The reslope option allows you to make small corrections to the calibration curve using a single standard to compensate for minor changes in instrument conditions A reslope standard near the middle of the calibration range usually gives the best results To enter the concentration of a reslope solution touch this field to display the Reslope dialog Enter the required concentration and then touch OK Reslope would appear in Analyze page as one of the standard selections when the appropriated standard calibration equation is selected If the calibration equation Through Zero had been selected Calibration Equation dialog in Calibration subpage The calibration equation describes the mathematical relationship between the absorbance reading and the concentration of the analyte in the solutions being measured Various calibration equations are available depending on whether the calibration curve is linear or non linear whether it passes through the origin or makes an intercept with the absorbance axis and on the technique of calibration used Nonlinear Through Select this option if you expect the concentr
217. t door closed when the flame is burning and never directly view the flame unless you are wearing UV absorbing glasses AAnalyst 200 User s Guide Acetylides If you have aspirated high concentrations of copper silver or mercury solutions into an acetylene flame unstable acetylides may have formed in the burner chamber If permitted to dry these compounds may explode i WARNING 1 Aspirate dilute acid 1 v v HCI solution for 5 minutes then aspirate with deionized water for another five minutes before turning off the flame 2 Extinguish the flame and allow the burner head to cool 3 Remove the burner head 4 Pour about 500 mL of deionized water slowly through the neck of the burner chamber to thoroughly flush the chamber and the drain system 5 Empty the drain vessel NOTE Dispose of hazardous or corrosive solutions properly and refer to your local safety regulations for proper disposal procedures Cyanide solutions If you intend to aspirate cyanide solutions make sure that the pH of the liquid in the drain vessel is greater than pH 10 toxic hydrogen cyanide gas is formed when cyanides contact acidic solutions e Never allow solutions containing cyanides to mix with acidic solutions Safety Practices Safety Conventions in the Hardware Guide Any of the following safety conventions can be used throughout this guide This is an example of a warning a situation that could lead to a personal injury WARNI
218. te button Print button External Keyboard checkbox 7 30 Use this button to close the dialog Changes made cannot be cancelled Click on this button and the message do you really want to do this appears If you click OK the sample information will be cleared Click on this button to opens the Open Sample Information where you can open a stored sample information file Click on this button to Open the Save Sample Information dialog where you can save the current sample information in a file Click on this button to open the Delete Sample Information dialog where you can delete the stored sample information files Click on this button to send the current sample information to the printer If turned on keyboard numeric entry dialogs are not displayed from this dialog text is typed directly into the entry fields AAnalyst 200 User s Guide Recommended Conditions You use this page to show the recommended analytical conditions for determinations using the flame technique The analytical conditions shown can often be used to produce acceptable results for determining elements in samples with a simple matrix Recommended Conditions Screen 7 18 Recommended Conditions Dialog 7 31 Touch Screens Network Dialog AAnalyst 200 data can be saved to a stand alone computer or to a network computer using a LAN connection Once a network connection is established all the analyses result data will automatically be saved
219. the center of the end cap Then release the spring clamp while you make sure the spring clamp slips over the nebulizer flange CAUTION Use care installing the nebulizer as the impact bead is quite fragile 7 Rock the nebulizer slightly to make sure it is set correctly in the end cap If excessive movement doesn t occur it is set properly 8 The nebulizer installation is complete 9 31 Maintenance Drain System Maintenance Drain system maintenance includes cleaning or flushing the drain system replacing the drain tubing and emptying the drain vessel when full Replacing the drain trap and switch assembly must be done by trained service personnel only The figure below shows all the parts of the AAnalyst 200 drain system The drain hose and vessel must be checked periodically for wear and or chemical attack The drain tubing should be clear with as few bends as possible The drain system should be replaced if it has deteriorated Spital Wrap g Drain Interlock Cable Connector at Bumer y Interlock Cable Drain Tubing Retainer Cap Drain interlock Jp Float Switch Assembly Drain v Loop Waste Vessel Figure 9 10 The burner drain system 9 32 AAnalyst 200 User s Guide Cleaning or flushing the Drain System It is recommended that the drain system be flushed thoroughly with water at the end of each working day to remove caustic corrosive or organic waste materials that could otherwise
220. tion subpage 7 18 startup tools dialOg eee eeeeeeeeeeeereeeneeeneee 7 28 Startup dialog oo eee eeeeeeeeeereeeneeenees 7 5 symbols on the instrument 2 9 T tenperat re Sirti o Gaede es 3 12 Salety e E E AT 2 12 through zero method addition zero 7 18 tools dialog description siirinsesi ii Aii 7 27 touch SCrEEN A ieee Mintle 6 19 installation ssis nisni ne 5 10 user interface components 6 20 7 4 1 8 troubleshooting cee eeeeeseeeseceneceeeees 10 3 burner problems eee eeeeeeeeeee 10 8 deuterium arc background corrector 10 13 flame analysis problems 10 4 flame problems ce eeeeeseeeeeeeee 10 8 lamp problems ccsccceesteeeeees 10 11 tubing acetylene supply seese 3 19 U units entry on Calibration subpage 7 17 unpacking Sp ctrome tei ennnen ann si 5 4 user interface components dialo gS oree seasea 6 20 7 4 parE Sri aeara Ee EE ree TENETE E 6 20 7 4 tabs isee e n 6 20 7 4 UV radiation Safety an a aiti 2 11 WwW warnings acetylene and Copper sseeeseeceeeeee 3 18 acetylene pressure 3 18 IL AE PATEE E ATAT 3 17 nitrous Oxide seene 3 17 waste disposal ceeeeeeeeeseeeeeeeeeeeees 2 21 contents of waste containers 2 21 defective lamps sssssesssesssessseessee 2 21 wavelength eeens eraa aesr i ai 7 7
221. to clean the capillary holder e The first simplified way should be used if the nebulizer is not difficult to clear This method involves simply passing one of the cleaning wires supplied through the capillary holder e The second complete procedure requires shutting down the spectrometer removing the nebulizer from the end cap and replacing the capillary tubing This procedure must be performed if you have no success with the first method Simplified Cleaning Procedure For AAnalyst Nebulizer For simplified light cleaning of a standard the AAnalyst nebulizer capillary holder proceed as follows 1 Unscrew the capillary tubing from the nebulizer 2 Take one of the cleaning wires P N 0303 0135 supplied and push it through the capillary holder from its wider open end It may take several attempts to pass the wire through the nebulizer 3 Repeat step 2 several times Then replace the capillary sample tubing 9 36 AAnalyst 200 User s Guide 4 Run one or more standards to determine if the capillary holder has been cleared If it has been cleared proceed with normal spectrometer operation otherwise proceed with the next procedure Complete Cleaning Procedure of AAnalyst Nebulizer To clean a stubborn blockage from the nebulizer perform the procedure below Wear protective gloves when you remove the nebulizer from the end cap if you were analyzing toxic samples WARNING Removal and Disassembly the Nebuliz
222. to establish your calibration curve before analyzing samples This procedure will analyze your blank and standards only 1 Touch the Calibrate button on the Analyze Sample screen A green light indicates that it has started 2 Touch the Display Calibration button to view the standard calibration curve 8 19 NOTE NOTE Analyzing Samples amp ee Screen 8 11 Display Calibration screen When you are satisfied with your calibration curve you may proceed to the next step Analyze Samples Use this step to analyze samples only 1 Touch the Analyze Samples button to begin analyzing samples A green light indicates that it has started 2 Touch the Display Calibration button to view the calibration curve at anytime during the run 3 Proceed to the next step To stop analyzing samples at anytime touch the Analyze Sample button to turn the function off Analyze All This step will start analyzing your entire run blank standards and samples 1 Touch the Analyze All button to begin your run A green light indicate that it is has started 2 Touch the Display Calibration button to view the standard calibration curve at anytime during your run To stop the run touch the Analyze All button to turn the function off If you were in the middle of running your samples and would like to continue the run you must change the parameter of First Sample Location on the Analyze Samples page to the desired sample location then t
223. tylene outlet gauge pressure is below these values Air supply requirements For the burner system an air supply that is clean dry and oil free is required The air supply should provide a minimum of 28 liters min 1 cubic foot min at a minimum pressure of 300 kPa 44 psig The air supply should be suitably filtered to remove oil water and solid particles Air compressor A small oil less air compressor meeting the air supply requirements is available from PerkinElmer The use of an air dryer filter is strongly recommended to remove entrained water oil water aerosols and solid particles from compressed air lines Water in the air supply can cause severe damage to the pneumatics 3 16 AAnalyst 200 User s Guide Risk of damage to the instrument CAUTION Water in the air supply can cause damage to the pneumatics Use only dry air Bleed compressor tanks to remove water at least once a week Air compressors are generally uncomfortably noisy to have in the immediate vicinity of the instrument Whenever possible locate them at some distance from the laboratory in an area providing suitable ventilation Air cylinders Cylinders of compressed air can also be used but are recommended only as an emergency or short term solution A standard 1 size air cylinder will last only about five hours It is common to find other than 20 oxygen in air cylinders This can cause erratic burner operation and non reproducible analytical resu
224. ubing replacing the drain 9 30 vessel and interlock ceeeeeeeeeees 5 20 drain trap maintenance checklist eeseeeeeeeee 9 9 drain tube maintenance checklist eee 9 9 drain vessel maintenance checklist eee 9 9 drainage burner chamber cccscceseeceereees 9 32 E E Box removing 9 40 PEPlaCiNg wean waa 9 42 switches and connectors 00 5 24 EDL see lamp iosi erecri sorone 4 9 EDL 1 CONMECHON a ee a aA s 5 24 EDL 2 COnnection ssssssessssessssssesrseessssssesrsets 5 24 EDL see electrodeless discharge lamp 6 22 electrical Installation oes eeeeeeeeeereeeeees 5 23 installation category 3 20 pollution degree s es 3 20 safety ss wituinicareienla a R EE Eaa 2 13 electrical supply CONNEC UN Siirtotarrat iiene 4 19 grounded outlet 4 20 line COrdS niceties eaeteos cake eee 4 20 SPECIFICATIONS 0 eee eee eseeene eee ceeeees 4 19 supply voltage 4 19 volt amps rating seese 4 19 voltage regulator 4 19 electrodeless discharge lamp Installing en nean 6 22 electrodeless discharge lamp see lamp 4 9 element irnir ekien nian ns 7 7 dialog in Lamp page scese 7 7 VAMP E sel scndbbacesdtes 7 9 entry fields ANALYZE PALES cncaro reniir 7 24 emergency Shutdown eeeeeeeeeeeees 8 32 Emission Mode overview 0 000 8 23 environment operating conditions 2 18 environmental conditions preparing your lab sser 3 4 ethernet connect
225. ure 5 C to 40 C 41 F to 104 F e Relative humidity 20 to 80 without condensation e Altitude in the range 0 m to 2 000 m sea level to 6 562 feet Storage conditions e Ambient temperature 20 C to 60 C 4 F to 140 F e Relative humidity 20 to 80 without condensation Altitude in the range 0 m to 12 000 m sea level to 39 370 feet 2 18 AAnalyst 200 User s Guide Exhaust Venting Toxic combustion products metal vapor ozone etc can be generated by the system depending on the type of analyses being performed e You must provide an efficient exhaust venting system to remove toxic products generated during instrument operation 2 19 Safety Practices Safe Handling of Chemicals Some chemicals used with the instrument may be hazardous or may become hazardous after completion of an analysis The responsible body must take the necessary precautions to ensure that the surrounding workplace is safe and that instrument operators are not exposed to hazardous levels of toxic substances chemical or biological as defined in the applicable national state and local health and safety regulations and laws Venting for fumes and disposal of wastes must be in accordance with all national state and local health and safety regulations and laws 2 20 AAnalyst 200 User s Guide Decontamination Before using any cleaning or decontamination methods except those specified by PerkinElmer res
226. us concentrations Disposing of defective lamps Hollow cathode lamps and electrodeless discharge lamps contain small quantities of the lamp element in a very pure form If a lamp containing toxic elements becomes defective or otherwise unusable you must treat it as hazardous waste and dispose of it accordingly A licensed company in the chemical waste disposal business can provide lamp disposal in accordance with environmental regulatory requirements Please note that PerkinElmer does not take back lamps for disposal In addition hollow cathode lamps and deuterium lamps are maintained under reduced pressure Handle and dispose of them correctly to minimize the implosion risk For information the quantities of analyte material contained in the cathodes of hollow cathode lamps are listed in the table below Quantity of Material in Single Element Hollow ulti Element Hollow Cathode Lamps Cathode Lamps As Au B Ba Be Ca Dy Er Na K Pt Ru Eu Ga Gd Ge Hf Ho In Ir K La Li Mg Na Nd Pd Pr t Re Rh Ru Sc Se Sm Sn a Tb Tm Yb Y g Al Bi Cd Co Cr Mn a Mg Ca Zn Ag Au Mo Ni Sb Si Sr Te V W Sn Te Ca Mg Zn Ca Mg Al ose u Fe Hg Nb P Pb Ti Tl all other multi element HCLs For EDLs the quantity of analyte material used is much less than the quantities used in HCLs Typically only several milligrams of material are placed in the EDL bulb No PerkinElmer EDLs System 1 or 2 contain mo
227. ut This Manal ciccccccciscsssccasasseaccvasssacadarscacasesstcdcdvasseacavarabacanabacacasaeasecas 1 3 Conventions Used in this Manual ccccccceccccccccccessssesesccccessseneaeseeeess 1 5 Warning Labels on the Instrument eee ceeceseeeeceeeeeseeeeeeeeaeeeaeeeaaeenaees 1 6 Chapter 2 Safety Practices Chapter OVerview cess escevshssactevestifeshsdsigeesenecche bhanetan EEE E bec recess dae 2 3 Working Safely with the AAnalyst 200 00 cece ceeceeeeeeeeeeeeeeaeeeseeeaeenaeens 2 4 PreCautlons fai ise eee de eee nee saat ls ete re el ee 2 5 Hazards with Flame Atomization eee eeeeeeseeeneeeneeeseecnseceseceaeceseeneeeees 2 6 Safety Conventions in the Hardware Guide eee ceeceeceeeeeeeeeeeeeeeeeenes 2 8 Symbols Used on the Instrument eee eeseceseceseceseceeceeeeseceseesseeeeneeeaes 2 9 Safety Practices for Flame Atomization cee eeceeeeeeeeeneeeeeereeeeeenaees 2 10 High Temperatures neeesa E E E E EERE 2 12 Electrical Safety insisi ina aa E pei 2 13 Compressed Gase Sines tease Soave esa eenia a AE E EENE EES 2 14 Safe Handling of Gas Cylinders 0 eee cesceseceeeceeeeeeeeeeeeeeaeeeaeeeaaeenaees 2 15 Operating Conditions isee oeieo niie e aai a e a aa 2 18 Exhaust Venting scciehsiectatecg2bi ste veal beancodt o ioei EEEE ETE OE E EE a 2 19 Safe Handling of Chemicals cecesceseceseceseceeeceeeeeeeeeeeeeeaeeeaeeeaaeenaees 2 20 Decontamination drieen nion arrn a A E eE E A Saa 2 21 Waste Disposal aa en e atau A AE
228. w T R X my D S D I N IN N Screen 8 5 Parameter page Spectrometer subpage On Parameters page Calibration subpage Select the Calibration Equation 1 For this example select Linear Through Zero Enter mg L for Units On Parameters page Calibration subpage Standard Concentrations section 1 Enter the concentration of the first standard for the element that you are determining e g 0 5 for copper 2 Enter the concentration of Standard 2 for the element you are determining e g 1 0 for copper 3 Enter the concentration of Standard 3 for the element you are determining e g 1 5 for copper For the above example we will only be calibrating with 3 standards 8 12 AAnalyst 200 User s Guide Calibration breton Calibration Equation jLinear Through Zero 4 Units mg L Calibration Standard Concentrations Figures After Decimal 3 4 0 500 5 2 1 000 6 3 1 500 a S G O Reslope 1 000 Screen 8 6 Parameter page Calibration subpage GT LAS A E E AE A de E E A A Lod F 3 C a s A C 1 C Parameter entry is now complete Proceed to the next step Analyze samples As measurements are made the results appear on the Analyze screen You may view the calibration curve of the analyses at anytime by touching the calibration curve button Screen 8 7 Display Calibration screen 8 13 NOTE NOTE NOTE Analyzing Samples Touch the Analyze tab to d
229. y and see the pressure indicators 3 14 AAnalyst 200 User s Guide Recommendations for compressed gas systems Gas installations Legibly mark gas lines and outlets to clearly identify the contents Use the chemical name or commercially accepted name for the gas Use only approved regulators tubing and hose connectors Arrange gas hoses where they will not be damaged or stepped on and where things will not be dropped on them Check the condition of pipes hoses and connectors regularly and replace any damaged parts Perform periodic gas leak tests at all joints and seals of the gas system by applying an approved gas leak detection fluid Using gas cylinders Store cylinders in accordance with the applicable national state and or local regulations and standards Legibly mark cylinders to clearly identify the contents and status full or empty Use the chemical name or commercially accepted name for the gas When gas cylinders are stored in confined areas such as a storage room make sure that ventilation is adequate to prevent toxic or explosive accumulations of gas Do not store acetylene in close proximity to oxidizing gases such as nitrous oxide Store all gas cylinders upright with the valve cap in place in a dry well ventilated area protected against temperature extremes Do not locate gas cylinders near exits and exit routes elevators gangways or in locations where heavy moving objects may strike or fal
230. you intend to analyze samples containing organic solvents The atomizer compartment door is closed The pH of the liquid in the drain vessel is greater than pH 10 if you intend to aspirate cyanide solutions Do not leave the flame unattended Always make sure that there is a fire extinguisher near the instrument Never change the gas pressure or shut a gas valve while the flame is burning Do not allow the burner head slot to become blocked This can cause a flashback of the flame Do not place open containers of flammable liquids and solvents near to the flame Be especially careful with samples that contain highly volatile solvents When you have analyzed samples containing organic solvents flush all traces of solvent from the burner system The drain system 2 10 Always place the drain vessel in a well ventilated place underneath the spectrometer in full view while you are working with the spectrometer This prevents the build up of potentially hazardous gases and allows you to see the liquid level Empty the drain vessel frequently especially do not allow the drain vessel to fill with organic solvent Thoroughly flush the drain system as described in the guide when you shut down the system Check the condition of the drain tube regularly especially if you use organic solvents Replace the drain tube when it first shows signs of cracking or discoloration AAnalyst 200 User s Guide UV radiation You should be awa
231. you perform any maintenance or installation procedures follow the instructions in the guide exactly e Do not attempt to service the gas control system yourself A PerkinElmer service engineer or similarly authorized and trained person must perform the work When you shut down the instrument for example at the end of the working day shut all the gas lines at the cylinder or regulator valves Bleed the lines between the regulator and instrument to atmosphere before switching off the exhaust venting system Warning Flashback Hazard PerkinElmer burner systems are designed for use with compressed air The use of oxygen can cause an explosion in the burner system And oxygen enriched air can cause a flashback of flame WARNING Never use oxygen or oxygen enriched air with PerkinElmer burner systems Use only compressed air 2 17 Safety Practices Operating Conditions Warning Explosive Atmosphere This instrument is not designed for operation in an explosive atmosphere WARNING Recommended operating conditions e Indoors The location must be free of smoke dust corrosive fumes direct sunlight and excessive vibration e Temperature 15 C to 35 C 59 F to 95 F Maximum rate of change not exceeding 3 C 5 F per hour e Relative humidity 20 to 80 without condensation e Altitude in the range 0 m to 2 000 m sea level to 6 562 feet Safe operating conditions e Indoor e Temperat
232. yst 200 Laboratory requirements for the instrument are reviewed in this chapter Chapter 4 System Description This chapter contains information on the components of the AAnalyst 200 how it works and instrument specifications Chapter 5 Installation Information on installing and re installing your AAnalyst 200 should you ever need to move your system is provided Chapter 6 Setting Up Instrument Detailed information on how to align adjust and optimize the AAnalyst 200 is provided in this chapter Chapter 7 Touch Screens Detailed information on how to operate the AAnalyst 200 using the touch screen is provided in this chapter Chapter 8 Preparing for an Analyses Detailed information on how to set up the AAnalyst 200 for analyses is provided in this chapter Chapter 9 Maintenance Maintenance and cleaning procedures for the various components of your AAnalyst 200 are provided 1 3 Introduction Chapter 10 Troubleshooting Performance checks troubleshooting information software and system error messages are provided for the AAnalyst 200 1 4 AAnalyst 200 User s Guide Conventions Used in this Manual Normal text is used to provide information and instructions Bold text refers to text that is displayed on the screen All eight digit numbers are PerkinElmer part numbers unless stated otherwise Notes cautions and warnings Three terms in the following standard formats are used to highlight special circumsta
233. ze the System V Calibrate the Specrtrometer i Analyze the Samples EALA N Lamp Flame Page Page Ne S Analyze Page a S Analyze Page g 1h G h Figure 8 1 Sequence of operation chart Analyzing Samples Manual Flame Analyses Overview Once the system has been powered up and optimized analyzing samples is simply a matter of entering parameters then aspirating solutions of a blank standards and samples The AAnalyst 200 has the capability to use up to eight calibration standards and a choice of calibration equations An example of an aspirating sequence for linear calibration is shown below Blank 4 Standard 1 Standard 2 Standard 3 4 Sample 1 Sample 2 4 Recalibrate or Reslope 4 Sample 3 Sample 4 etc For nonlinear zero intercept or linear zero intercept calibration you can aspirate a reslope standard at any point after the first sample is run This section contains an example of how to run Flame AA analyses manually using linear nonlinear and analyte additions techniques The examples take you step by step through the required procedures AAnalyst 200 User s Guide Analyzing Samples using Linear Non Linear Calibration The following example describes how to run samples using the linear calibration technique It should be noted that the same steps are carried out when using the nonlinear calibration te

AAnalyst 200 User's Guide

Contents

Download Pdf Manuals

Related Search

Related Contents