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PerkinElmer aanalyst 200, User Manual

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Analyzing Samples

 

8-4   

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 

↓

 

Standard 1 

Standard 2 

Standard 3 

↓

 

Sample 1 

Sample 2 

↓

 

Recalibrate or Reslope 

↓

 

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. 

Summary of Contents for aanalyst 200

Page 1: ...AAnalyst 200 User s Guide ...

Page 2: ...antability 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 whatsoe...

Page 3: ...Venting 2 19 Safe Handling of Chemicals 2 20 Decontamination 2 21 Waste Disposal 2 22 Electromagnetic Compatibility EMC 2 23 WEEE Instructions for PerkinElmer Products 2 24 References for Laboratory Safety Practice 2 25 Chapter 3 Preparing Your Laboratory Introduction 3 3 Environmental Conditions 3 4 General Laboratory Requirements 3 5 Location and Space Requirements 3 7 Exhaust Vent Requirements ...

Page 4: ...ing up the Burner System 6 5 Installing Solvent Resistant Components in the Burner 6 11 User Interface 6 19 Installing Lamps 6 21 Switching on the Spectrometer 6 25 Safety Checks 6 26 Using the Background Corrector 6 27 Optimization Procedures 6 28 Aligning Lamp 6 29 Setting the Burner Height 6 33 Igniting the Flame 6 35 Preadjusting the Nebulizer 6 37 Optimizing the Burner System 6 39 Rinsing the...

Page 5: ...ning the Burner System 9 17 Cleaning the Burner Head 9 19 Pre Conditioning a New Burner or Drain Tube 9 21 Removing the Burner Head 9 22 Removing the Burner Assembly from the Instrument 9 23 Disassembling the Burner Chamber 9 25 Reassembling the Burner System 9 28 Drain System Maintenance 9 32 Cleaning the Nebulizer 9 36 Replacing Parts of Wear 9 45 E Box 9 46 Maintaining the Acetylene Supply 9 50...

Page 6: ......

Page 7: ...Introduction 1 ...

Page 8: ......

Page 9: ... 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 ...

Page 10: ...Introduction 1 4 Chapter 10 Troubleshooting Performance checks troubleshooting information software and system error messages are provided for the AAnalyst 200 ...

Page 11: ... used to highlight special circumstances and warnings NOTE A note indicates additional significant information that is provided with some procedures CAUTION We use the term CAUTION to inform you about situations that could result in serious damage to the instrument or other equipment Details about these circumstances are in a box like this one WARNING We use the term WARNING to inform you about si...

Page 12: ...Introduction 1 6 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 ...

Page 13: ...fore servicing C WARNING UV Light Source Wear protective glasses when working with this cover removed D Nebulizer clamp must be lowered and locked over the nebulizer flange E Never use oxygen Read instructions before lighting burner Drain trap must be filled F WARNING Hot surfaces G Emergency flame off switch ...

Page 14: ...Introduction 1 8 Figure B Label located on the right side of the AAnalyst 200 A CAUTION do not restrict air intake or exhaust ...

Page 15: ...00 User s Guide 1 9 Figure C Labels located on the back of the AAnalyst 200 C D A B E Burner Gases Connections For more information see page 5 14 N2O blue hose Air black hose C2 H2 red hose Purge translucent hose ...

Page 16: ...el of the AAnalyst 200 A Turn the power switch off and unplug the AC line cord from the AC outlet before loosening the screw B WARNING Grounding circuit continuity is vital for safe operation of equipment Never operate equipment with grounding conductor disconnected ...

Page 17: ... WARNING To prevent a shock hazard turn the power switch off and unplug the AC line cord from the AC outlet C 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 ...

Page 18: ...Introduction 1 12 ...

Page 19: ...Safety Practices 2 ...

Page 20: ......

Page 21: ...cy 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 supplied with the AAnalyst 200 and accessories before you start working with the instrument Carefully read the safety information in this chapter and in the o...

Page 22: ...ts 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 received adequate training If the instrume...

Page 23: ...nalyst 200 Be sure that the voltage of the AAnalyst 200 corresponds to the power line voltage used in your laboratory Never remove the side panels of the AAnalyst 200 without shutting down the instrument and disconnecting the instrument power cord from line power Only high quality purge gases should be used with the AAnalyst 200 Minimum purity of 99 9 is recommended A high quality filter dryer acc...

Page 24: ...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 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 t...

Page 25: ...low 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 ...

Page 26: ...d 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 CAUTION We use the term CAUTION to inform you about situations that could result in serious damage t...

Page 27: ... 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 on position of the main power switch Indicates the protective conductor terminal Indicates the off position of the main power switch ...

Page 28: ...ad 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 Always place the drain vessel in a well ventilated pl...

Page 29: ...n do not remove any covers unless specifically instructed to do so in the guide or you may be exposed to potentially hazardous UV radiation Always wear UV absorbing eye protection when viewing The flame especially the nitrous oxide acetylene flame Hollow cathode or electrodeless discharge lamps The deuterium background correction lamp ...

Page 30: ... 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 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 ...

Page 31: ... 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 Connect the instrument to a correctly installed line power outlet that has a protective conductor connection earth ground Do not operate the instrument with any covers or internal parts removed Do ...

Page 32: ...ation on the potential hazards associated with the gas WARNING Warning Nitrous oxide is a strong oxidant and an asphyxiant 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 materials Store nitrous oxide cylinders in a well vent...

Page 33: ...safety practices for the proper identification storage and handling of gas cylinders Consult the following references for more detailed information and additional guidelines Compressed Gas Association USA Safe Handling of Compressed Gases in Containers pamphlet no P 1 1984 Compressed Gas Association USA The Inert Gases Argon Nitrogen and Helium pamphlet no P 9 1992 Identification of Gas Cylinders ...

Page 34: ...y 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 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 Use only regulators tubing and hose connectors approved by an ap...

Page 35: ...st fluid When you perform any maintenance or installation procedures follow the instructions in the guide exactly 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 valv...

Page 36: ... 95 F Maximum rate of change not exceeding 3 C 5 F per hour Relative humidity 20 to 80 without condensation Altitude in the range 0 m to 2 000 m sea level to 6 562 feet Safe operating conditions Indoor Temperature 5 C to 40 C 41 F to 104 F Relative humidity 20 to 80 without condensation Altitude in the range 0 m to 2 000 m sea level to 6 562 feet Storage conditions Ambient temperature 20 C to 60 C...

Page 37: ...g Toxic combustion products metal vapor ozone etc 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 ...

Page 38: ...sary 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 l...

Page 39: ...rrying 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...

Page 40: ...nusable 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 the...

Page 41: ... 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 NOTE Changes or modifications not expressly approved by PerkinElm...

Page 42: ...ting 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 W...

Page 43: ...n 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...

Page 44: ...Safety Practices 2 26 ...

Page 45: ...Preparing Your Lab 3 ...

Page 46: ......

Page 47: ...s shown in the following checklist need to be considered when preparing the laboratory for the instrument Environmental Conditions General Laboratory Requirements Laboratory Space Requirements Exhaust Vent Requirements Gas Supply Requirements Electrical Requirements Lamps Make sure your laboratory meets all of the requirements before you begin to install the system ...

Page 48: ...lame 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 fla...

Page 49: ... 15 C to 35 C 59 F to 95 F Maximum rate of change not exceeding 3 C 5 F per hour Relative humidity 20 to 80 without condensation Altitude in the range 0 m to 2 000 m sea level to 6562 feet Safe operating conditions Indoor Temperature 5 C to 40 C 41 F to 104 F Relative humidity 20 to 80 without condensation Altitude in the range 0 m to 2 000 m sea level to 6562 feet Storage conditions Ambient tempe...

Page 50: ...y 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 wh...

Page 51: ...st 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 Make sure that there is space at the rear and sides of the system for air to circulate freely Do not block the fan operating on the right side of the instrument Make sure that there is sufficient room for you to work comfortably...

Page 52: ...Preparing Your Lab 3 8 473 mm 650 mm 910 mm 700 mm 760 mm 170 mm Figure 3 1 Outside dimensions of instrument ...

Page 53: ...ries 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 ca...

Page 54: ...Preparing Your Lab 3 10 Approx 170 mm 525 mm 700 mm Figure 3 2 Space requirements for the spectrometer system front view ...

Page 55: ...AAnalyst 200 User s Guide 3 11 Figure 3 3 Space requirements for the spectrometer system top view ...

Page 56: ...ront bearing To withstand these temperatures stainless steel tubing must be used NOTE 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 stainle...

Page 57: ...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 o...

Page 58: ...dapter 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 10 cm 4 in 15 cm 6 in 30 cm 12 in 11 cm I D 4 3 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 safet...

Page 59: ...s 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 e...

Page 60: ...ARNING Warning Acetylene Explosion Hazard Acetylene can decompose explosively at pressures higher than 103 kPa 1 03 bar 15 psig Αlways make sure that the acetylene 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 pr...

Page 61: ...used it is important to specify compressed air rather than breathing air and that the oxygen content is less than 20 WARNING 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 enriched air with PerkinElmer burn...

Page 62: ...ous oxide pressure regulator is available from PerkinElmer Acetylene supply requirements WARNING 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 these values Acetylene can react with copper to form a readily explosive compound Never use copper tubing or fittin...

Page 63: ...iron fittings may also be used Cast iron fittings cannot be used safely for acetylene lines Safe use of acetylene Periodically check for the presence of acetylene in the laboratory atmosphere especially near the ceiling Never allow the outlet gauge pressure to exceed 103 kPa 1 03 bar 15 psig acetylene can explode spontaneously above this pressure Prevent acetylene from coming into contact with cop...

Page 64: ...he 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 a...

Page 65: ...n 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 ...

Page 66: ...Preparing Your Lab 3 22 ...

Page 67: ...System Description 4 ...

Page 68: ......

Page 69: ... 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...

Page 70: ... 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 ...

Page 71: ...tomizer compartment Τhe 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 burner system 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 pe...

Page 72: ... 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 ...

Page 73: ...reduced setup times for easy and accurate operation Lumina Hollow Cathode Lamp Socket Plug Figure 4 3 Drawing of a Lumina hollow cathode lamp 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 fo...

Page 74: ...ded Universal Adapter Cable for the Coded Intensitron HCL s N305 0196 Figure 4 4 The Intensitron hollow cathode lamp with universal 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 Adapter Cable for the Non coded Intensitron HCL s N305 0197 Intensitron Hollow C...

Page 75: ...with the AAnalyst Instruments Note Use this coding plug with the Instruments AAnalyst 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 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...

Page 76: ...ess 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 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 ...

Page 77: ... 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 signals as large as 3 absorbance units The background corrector is internally installed with its power supplied from the ...

Page 78: ...nd 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 Nebulizer Burner chamber including the flow spoiler and end cap Burner head Drain system Gas control system incorporated in the spectrometer Flow Spoiler Drain Burner Head End Cap Burner Mixing Chamber Nebulizer Side Arm Nebulizer Bod...

Page 79: ...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...

Page 80: ...er 0303 0204 117V 0303 0349 230V Nitrous Oxide Hose Assembly 0047 0258 Male Connector 0990 3946 1 4 in Pipe to 5 16 in Compression Fitting Air Supply Air Dryer Filter 0047 0652 or Air Acetylene Filter N930 1398 5 16 in Compression Fitting Adapter 0990 3215 CGA No 300 or 510 Acetylene Hose Assembly 0057 0559 Air Argon Hose Assembly 0057 0567 Acetylene Regulator 0303 0106 Acetylene Tank Nitrous Oxid...

Page 81: ...n the nitrous oxide burner head N040 0102 10 cm single slot burner head for air acetylene operation standard with all burners 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 N040 0102 10 cm 4 in Air Acetylene Operation N040 0103 10 cm 4 in 3 Slot Air Ac...

Page 82: ...s 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 po...

Page 83: ...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 installing the nebulizer on the burner checking that the burner end cap is secure connecting and securing the gas ho...

Page 84: ...u consult the troubleshooting information included in this manual before you call a PerkinElmer service engineer Refer to Chapter 10 Troubleshooting 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 ...

Page 85: ...oltage 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 th...

Page 86: ... 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 NEMA 5 15 0998 8986 Europe CEE 7 Schuko 0999 1415 Europe Switzerland 0999 1413 Europe Italy 0999 1422 Old British Standard BS 546 India 0999 1423 British Standard BS 1363 United ...

Page 87: ...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 heated to dissociate the hydride gas into free atoms or in the case of mercury ...

Page 88: ...s 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 Quartz Cell Burner Head Bu...

Page 89: ...Installation 5 ...

Page 90: ......

Page 91: ...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 Inspect the shipment 2 Unpack the spectrometer 3 Place the spectrometer on the bench 4 Install the touch screen 5 Connect the gas hoses 6 Set up the burner system 7 Install the burner door 8 Ins...

Page 92: ...mizer 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 bo...

Page 93: ...AAnalyst 200 User s Guide 5 5 Carton Sleeve Shipping Carton Top Cardboard Boxed Items as required Shipping Carton Base Molded Foam Padding Figure 5 1Exploded view of the shipping carton ...

Page 94: ...he bench should be nearby 2 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 3 With knees bent simultaneously lift the instrument out of the carton as you rise to a standing position Carefully place the instru...

Page 95: ...ide 5 7 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 ...

Page 96: ...ist 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 ...

Page 97: ...Nebulizer tubing 300mm for manual sampling 1 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 Form 1 0993 6643 AAnalyst 400 Safety Booklet 1 0943 2046 Software Utilities CD 1 0993...

Page 98: ...moving lamp door Remove 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 locatio...

Page 99: ... 5 11 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 Screen 5 1 Slot above the lamp compartment ...

Page 100: ... 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 ...

Page 101: ...e to the E Box s Display Connector receptacle 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 E Box Display Connector ...

Page 102: ...ax 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...

Page 103: ...pply WARNING 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 ...

Page 104: ...lter 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 ...

Page 105: ...n 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 If you 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 ...

Page 106: ... and gas hoses regularly for leaks using a suitable leak testing fluid Acetylene regulator Acetylene cylinder Red acetylene hose from spectrometer Flash arrestor Figure 5 8 Acetylene supply connections 1 Connect the red acetylene hose coming from the back of the spectrometer to the acetylene regulator 2 Tighten the connection using the double wrench technique Hold the fitting on the air dryer filt...

Page 107: ...AAnalyst 200 User s Guide 5 19 Setting up the Burner System Figure 5 9 Full view of the AAnalyst 200 Instrument ...

Page 108: ...sel 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 th...

Page 109: ...r 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 ...

Page 110: ...ou 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...

Page 111: ...tact your local PerkinElmer office for advice 2 Make sure that the On Off switch on the spectrometer s E Box behind the lamp door is in the Off position depressed 3 Pass line cord receptacle underneath through the slot at the bottom of the lamp compartment 4 Insert the line cord receptacle into the line power input module on the E Box 5 Insert the line cord plug into a suitable electrical outlet 6...

Page 112: ...ut Figure 5 12 Switches and ports on the front panel of the E Box Autosampler Connection port for autosampler Serial 1 Connection for serial port Ethernet Connection port for the network Remote Trigger Connection port for foot switch or FIAS Read cable EDL 1 Connection port for EDL in lamp position 1 EDL 2 Connection port for EDL in lamp position 2 Printer Connection port for printer Keyboard Conn...

Page 113: ...ecting autosampler AS 90 plus or AS 93 plus to the E Box 1 Connect RS 232 cable to 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 Ch...

Page 114: ... 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 E Box Remote Trigger Foot Switch Figure 5 14 Foot Swi...

Page 115: ...Operation of the Instrument 6 ...

Page 116: ......

Page 117: ... 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 Gas Purge clear line ...

Page 118: ...commended A high quality filter dryer accessory is recommended for the removal of any moisture from the purge gas WARNING 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 valve ...

Page 119: ...r 3 If you want to use an impact bead or spacer on the nebulizer make sure that it is correctly installed 4 If you intend to aspirate organic solvents use a yellow color drain tube that is designed for organic solvents 5 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...

Page 120: ...r Nebulizer Side Arm Nebulizer Body Spacer Impact Bead Structure O Rings 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...

Page 121: ...u ll connect the nebulizer oxidant hose to the nebulizer side arm Remove the plastic nut from the 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 6 Slide the NEB oxidant tubing onto the ridges on the nebulizer side arm 7 Using the Apiezon grease lightly lubricate the OUTSIDE of the tubing where the nut ...

Page 122: ...rews 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 Figure 6 3 Checking that the burner end cap is secure ...

Page 123: ...ar 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 Tighten the compression fitting hand tight plus a turn using two wrenches one wrench to hold the nebulizer fitting and the other to turn the compression fitting The third h...

Page 124: ...ead 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 chambe...

Page 125: ...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 d...

Page 126: ...Operation of the Instrument 6 12 Installing the Burner Mount Assembly Figure 6 6 Installing the burner mount assembly ...

Page 127: ...ace 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 Warning Flashback While the flame is on DO NOT push the lever that is located on the burner mount assembly ...

Page 128: ...nnecting 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 the drain tubing and pour approximately 250 mL of water into it until you hear the water start to drip into the vessel ...

Page 129: ...t 200 Atomic Absorption Spectrometer Retainer Cap Interlock Cable Waste Vessel Drain interlock Float Switch Assembly Drain Loop Drain Interlock Cable Connector at Burner Spiral Wrap Drain Tubing Figure 6 7 Installing the burner drain system ...

Page 130: ...tlet on the burner end cap Tighten the drain clamp 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 ...

Page 131: ...he drain tubing 3 Reconnect the drain tubing to the burner end cap 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 pus...

Page 132: ...Operation of the Instrument 6 18 Figure 6 9 Installing the lamp compartment cover ...

Page 133: ...ains active areas that you touch to perform the required action You may find it more convenient to use a stylus or the 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 ...

Page 134: ...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 num...

Page 135: ...d corrector deuterium lamp D2 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 ...

Page 136: ...cket 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...

Page 137: ...o 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 o...

Page 138: ...ry touch the respective On Off box to switch off the lamp 6 Touch OK 7 Unplug and remove the lamp For EDLs remove the coding plug as well Tips for installing lamps Use PerkinElmer lamps Do not touch the front window of the lamp perspiration or other contamination can reduce intensity of the radiation With EDLs make sure that you use the correct coding plug and connect it to the receptacle on the l...

Page 139: ...r 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 spectrometer to complete initialization The Lamp page is displayed on the Touch Screen ...

Page 140: ...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 close...

Page 141: ...e 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 combine...

Page 142: ...y 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 The nebulizer Initially you must set the solution...

Page 143: ... 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 Αlways wear UV absorbing safety glasses when looking at the radiation from the lamps ...

Page 144: ...y display Align the lamp to obtain maximum energy Coded single multi element Lumina lamp 1 Start up the spectrometer but do not ignite the flame 2 Lamps Installed are automatically shown in the energy field box on the Lamp page The element entry field box automatically shows the element installed 3 Touch the Element entry field box on the Lamp page to display the Select Element dialog You select t...

Page 145: ... from the selected list Touch OK 3 Touch the Setup Instrument button on the Lamp page of the touch screen The recommended parameters for that element are automatically set up 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 4 Turn the tw...

Page 146: ...Install Lamps dialog 3 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 4 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 alternat...

Page 147: ...ly you need a lamp that emits a beam of visible radiation 3 If not already on power up the spectrometer Do Not Ignite The Flame 4 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 Figure 6 16 Locating the r...

Page 148: ...ion 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...

Page 149: ...e Chapter 8 for the procedure to follow after an emergency shutdown To ignite the flame 1 Start up the spectrometer system The power switch is on the E Box located behind the lamp door 2 Adjust the gas supply regulator pressure to the recommended values 3 Perform the safety checks 4 Touch the Flame tab to display the Flame page 5 Touch the Oxidant Tab to display the Flame Type dialog 6 Touch the b...

Page 150: ...ould appear uniform and stable throughout its length If it is not even after 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 WARNING When using nitrous oxide the fl...

Page 151: ... 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...

Page 152: ...ion 4 Turn the nebulizer regulator slowly counter clockwise until bubbles start to appear from the end of the sample tube in the standard solution 5 Then turn the nebulizer regulator 1 to 1 turns clockwise 6 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 regulato...

Page 153: ...liminary 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 1 Prepare a blank solution Use the same solvent as you use to prepare the s...

Page 154: ...ce reading Optimizing the nebulizer In this procedure you optimize the nebulizer aspiration rate for the solutions you will use in the subsequent analyses WARNING Warning Flashback Hazard When you optimize the nebulizer using a nitrous oxide acetylene flame 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 neb...

Page 155: ... 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 ...

Page 156: ...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 observing the continuous graphics display ...

Page 157: ... system Procedures If you used only aqueous solutions during the analyses Aspirate deionized water for 5 minutes If you used organic solvents during the analyses Aspirate for 5 minutes an organic solvent that is miscible with the samples that have just been aspirated Aspirate for 5 minutes methanol or another solvent that is miscible both with water and the solvent used previously Aspirate 1 v v n...

Page 158: ...Operation of the Instrument 6 44 ...

Page 159: ...Touch Screens 7 ...

Page 160: ......

Page 161: ...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 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...

Page 162: ...at 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 o...

Page 163: ... 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 ...

Page 164: ... 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 Screen 7 3 Lamp Setup Page ...

Page 165: ... Element 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 s...

Page 166: ... perform AGC AIC when you are setting up a lamp The system does this automatically for a lamp when you select Setup Instrument 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 Cont...

Page 167: ... 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 cu...

Page 168: ...required analyte element from the list in the dialog and the recommended parameters 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 ...

Page 169: ...phical absorbance display Screen 7 6 Flame Page To switch oxidant type 1 Shut off the flame and wait until the burner 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 If an air burner head is installed the Nitrous oxide option is...

Page 170: ...ene mixture with automatic changeover to nitrous oxide after a few seconds Oxidant Flow L min Touch entry field with associated arrow keys that displays the selected oxidant flow rate in liters min To change the flow rate you can either Touch the field to display the Oxidant Flow dialog and enter the required flow rate in this dialog or Touch the increase or decrease arrows the flow rate is change...

Page 171: ...ocks Screen 7 8 Interlock Dialog NOTE If air acetylene is used in place of N20 the N20 pressure interlock will be ignored and flame will light 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 ...

Page 172: ...arameters page This page comprises two subpages Spectrometer subpage 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 Screen 7 9 Spectrometer Subpage MHS Technique ...

Page 173: ...AAnalyst 200 User s Guide 7 15 Screen 7 10 Spectrometer Subpage Flame Technique ...

Page 174: ...hange 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 Print 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 Sample Handling When th...

Page 175: ...ield 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 Units 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 to...

Page 176: ... 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 th...

Page 177: ...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 Calculated Intercept Analyte Addition 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 u...

Page 178: ... 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 Dilution from the sample information file Screen 7 12 Analyze Samples Page Manual Data Disp...

Page 179: ...ple 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 c...

Page 180: ...e window touch this button Printer On Off 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...

Page 181: ...e numerical value are continuously updated to the current reading The analysis is limited to only one replicate per sample 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 abso...

Page 182: ...nd 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 Touch this entry field box to view the standard concentration dialog Use the dialog to select the standard concentration you want to analyze The st...

Page 183: ...the bottom of the Results Window 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 th...

Page 184: ...ill 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 This shows the name of the sample tray currently selected To select a different tray touch this entry field for tray dialog First Sample Location This shows the st...

Page 185: ...d 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 ...

Page 186: ... changed Network 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 Calibrate Stylus Touch this button to run a system utility to recalibrate the touch screen if the screens are not responding properly to you...

Page 187: ...le Sample ID Column Fill button Click on this button to open the Sample ID Column Fill dialog to 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 C...

Page 188: ...d sample information file Save button Click on this button to Open the Save Sample Information dialog where you can save the current sample information in a file Delete button Click on this button to open the Delete Sample Information dialog where you can delete the stored sample information files Print button Click on this button to send the current sample information to the printer External Keyb...

Page 189: ...e 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 Screen 7 18 Recommended Conditions Dialog ...

Page 190: ...ions for network computer Stand Alone Computer 1 Use a crossover cable P N 0941 0061 to connect the AA200 instrument to a computer Connect the crossover cable to the Ethernet port of the E Box see chapter 5 for connectors on the E Box 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 ...

Page 191: ...ter 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 name given to identify the stand alone computer To locate the computer name do the following procedure on the stand alone PC Point to the My Computer icon and right click the mouse once A shortcut menu appears and selects Prope...

Page 192: ... 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 Open Windows Explorer and right click on the desired drive or folder to make it sharable From the shortcut menu choose Sharing ...

Page 193: ...AAnalyst 200 User s Guide 7 35 Screen 7 22 Shortcut menu Properties folder appear and select Share this folder option ...

Page 194: ...Touch Screens 7 36 Screen 7 23 Properties dialog Click the Permissions button to set users permissions to the shared drive or folder ...

Page 195: ... not already have a user s name and password follow the procedure below Select Start Settings Control Panel The Control Panel dialog appears Double click Administrative Tools Computer Management The Computer Management dialog appears In the directory tree on the left of the Computer Management dialog drill down select System Tools Local Users and Groups Users From the Action menu select Action New...

Page 196: ...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 Double click on UserA A Properties dialog appears for UserA Click on the Member Of tab and then add UserA to the desired group using the Add button We will add UserA to the A...

Page 197: ... the AA200 Result Data folder Select Properties Click on the Security Tab Deselect Allow inheritable permissions from parent to propagate to this object 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 ...

Page 198: ...r for AA200 instrument 1 The ID can range from 0 255 For Static IP Network do the following Select Specify an IP address option on the Network dialog 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 Lo...

Page 199: ...d Requirement Computer running Windows NT 2000 or XP RS 232 female to female Serial Cable 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 Screen 7 28 Microsoft ActiveSync Inst...

Page 200: ...rial 1 of the E Box From the E Box run the RS 232 serial cable to the comport 1 2 3 or 4 of the computer Screen 7 29 Get Connected Window 4 From the AA application Touch Screen touch the Tools button to access the Tools dialog CAUTION Do not power off the instrument or disconnect the serial cable while downloading There is a slight risk of application failure to recover ...

Page 201: ...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 If the Partnership dialog appears select the No option button and then click Next Screen 7 31 New Partnership Dialog ...

Page 202: ... 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 4 A successful download w...

Page 203: ...cial 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 Use the arrow keys on the keyboard to Select Run or touch Run on the touch screen 6 Enter the word killer exe in the dialog box and touch OK NOTE Allow 10 seconds for Killer exe to terminate all ...

Page 204: ...Touch Screens 7 46 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 ...

Page 205: ...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 MSASYNC EXE file A dialog will appear indicating that MS Active Sync i...

Page 206: ...h 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 A green icon located on the lower right hand corner of the taskbar indicates successful connection ...

Page 207: ...ders stored on the AAnalyst 200 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 ...

Page 208: ...dow appears select the Delimited option and click Next 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 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 secti...

Page 209: ...AAnalyst 200 User s Guide 7 51 Screen 7 41 Test Import Wizard Step 3 21 Select Save As from the File menu to save your result as an excel file ...

Page 210: ...Touch Screens 7 52 ...

Page 211: ...Analyzing Samples 8 ...

Page 212: ......

Page 213: ... dialogs that you require for each step are shown Prepare Standards and Samples Startup and Prepare the System Enter Parameters Optimize the System Calibrate the Specrtrometer Analyze the Samples Lamp Page Install Lamps Dialog Flame Page Oxidant Dialog Parameters Page Spectrometer Subpage Calibration Subpage Lamp Page Flame Page Analyze Page Analyze Page Figure 8 1 Sequence of operation chart ...

Page 214: ...equations An example of an aspirating sequence for linear calibration is shown below Blank Standard 1 Standard 2 Standard 3 Sample 1 Sample 2 Recalibrate or Reslope 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 man...

Page 215: ... 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 7 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 ...

Page 216: ...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 fue...

Page 217: ...bpage 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 2 Enter the concentration of Standard 2 for the element you are determining e g 1 0 mg L for copper 3 Enter the ...

Page 218: ... view the calibration curve of the analyses at anytime by touching the display calibration button Touch the Analyze tab to display the Analyze page Touch the Printer On Off button if you wish the results to be printed 1 Run the blank Aspirate the blank solution Touch the Analyze Blank button 2 Run the standards Aspirate Standard 1 then touch the Analyze Standard button Aspirate Standard 2 then tou...

Page 219: ...ess the Analyze Sample button Aspirate Sample 2 and then press the Analyze Sample button NOTE 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 St...

Page 220: ...Analyzing Samples 8 10 Screen 8 4 Display Calibration screen ...

Page 221: ...nstrument 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 Integr...

Page 222: ... 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 calibr...

Page 223: ...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 ...

Page 224: ... 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 tou...

Page 225: ...se 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 Standard 8 Sample 1 Sample 2 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 i...

Page 226: ...le 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 ...

Page 227: ...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...

Page 228: ... 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 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 t...

Page 229: ...alyze screen in the order of the solutions analyzed The most recent results are displayed at the top of the screen Touch the Analyze tab to display the Analyze page Touch the Printer On Off button if you wish the results to be printed Calibrate Use this procedure to establish your calibration curve before analyzing samples This procedure will analyze your blank and standards only 1 Touch the Calib...

Page 230: ...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 NOTE To stop the run touch the Analyze All butto...

Page 231: ...AAnalyst 200 User s Guide 8 21 The results are displayed and printed Screen 8 12 Analyze page ...

Page 232: ...nt 4 Select the MHS technique from the startup screen or from the tools menu startup 5 Select or fill the required touch entry fields on the Parameters page Spectrometer subpage Screen 8 13 Parameters page Spectrometer subpage 6 Install and align the lamps that are required See chapter 6 for Aligning Lamps 7 Follow the procedures for setting up Flame Analyses including setting up and adjusting the...

Page 233: ...n Refer to the section on Standard Conditions in Analytical Methods for Atomic Absorption Spectrometry 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 Se...

Page 234: ...Analyzing Samples 8 24 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 ...

Page 235: ... 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 ...

Page 236: ...Analyzing Samples 8 26 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 ...

Page 237: ...AAnalyst 200 User s Guide 8 27 Screen 8 17 Flame page 8 Select the Parameters page Spectrometer tab Use the appropriate values to fill in the settings ...

Page 238: ...Analyzing Samples 8 28 Screen 8 18 Parameters page Spectrometer tab 9 Select the Parameters page Calibration tab In the Calibration Equation field touch the screen to access the dialog ...

Page 239: ... 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 ...

Page 240: ...age 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 Screen 8 21 Analyze page ...

Page 241: ...e Flame page 3 Touch the Flame On Off switch 4 The system uses a predetermined shutdown sequence to extinguish the flame safely NOTE 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 depressu...

Page 242: ...t off gases at source and bleed 3 Switch off the spectrometer at the operational on off switch on the front panel 4 If you 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 Remove the burner head Pour a large qu...

Page 243: ... all traces of these substances out of the system If the 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 Aspirate deionized water for 5 minutes If you used organic solvents during the analyses Aspirate ...

Page 244: ...Analyzing Samples 8 34 ...

Page 245: ...Maintenance 9 ...

Page 246: ......

Page 247: ...one 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 described in this chapter If additional maintenance is required contact a PerkinElmer Service Engineer CAUTION Before using any cleaning or decontamination methods except t...

Page 248: ...c substances and when measuring trace amounts of any elements Clean up spills immediately using a spill clean up kit approved by your organization WARNING In accordance with safe laboratory practices spilled material should be cleaned up and disposed of properly taking into consideration the following location and size of the spill chemical and physical properties of the material hazardous propert...

Page 249: ... if it is old If the 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 Normally the spectrometer optics will require little or no maintenance However low energy lamp readings or noisy or erratic results may indicate tha...

Page 250: ... dispersion characteristics of the grating and 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 ...

Page 251: ...f 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 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 Burner System Check for uneve...

Page 252: ...mponents are clean Fume ventilation Make sure that the main exhaust ventilation system functions correctly Always switch it on when you are using the instrument Environmental conditions Make sure that the environmental conditions are as described in Chapter 2 Spectrometer maintenance checklist External Surfaces Wipe over the surfaces with a lint free cloth moistened with a dilute solution of labor...

Page 253: ...flame may indicate that the slot needs cleaning See page 9 19 for cleaning procedure Check the width of the burner slot periodically Nebulizer If there is an obstruction in the nebulizer clear it using a copper cleaning wire Drain system Flush the drain system thoroughly at the end of each working day by pouring water down the neck of the burner chamber Drain vessel Empty the drain vessel regularl...

Page 254: ...s 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...

Page 255: ...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...

Page 256: ...ng 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 ...

Page 257: ...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 2 Aspirate methanol or another solvent miscible with both th...

Page 258: ...e compounds may explode 1 Aspirate dilute acid 1 v v HCl solution for 5 minutes before turning off the flame 2 Extinguish the flame and allow the burner head 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 ...

Page 259: ...ng the burner door 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 ...

Page 260: ...ner 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 ...

Page 261: ...f the nitrous oxide acetylene flame may cause deposits of pyrolytic carbon to build up along the burner slot WARNING 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 Warning Hydrochloric and Nitric Acids Risk of Burns Hydrochloric HCl and nitric HNO3 acids are corrosive and c...

Page 262: ... head slot is clean Check that the burner head is seated correctly Check the flow spoiler or impact bead for damage and replace any damaged parts 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 th...

Page 263: ... 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 bu...

Page 264: ...5 mm 0 020 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 Disca...

Page 265: ...ould 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 ...

Page 266: ...ner 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 Figure 9 4 Removing the burner head from the burner chamber ...

Page 267: ...ead 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 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 ...

Page 268: ...Maintenance 9 24 Figure 9 6 Removing the burner assembly from the instrument ...

Page 269: ...er 2 Unscrew the retaining ring Figure below and pull out the burner o ring 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 If you feel you ll need to completely remove the end cap from the chamber continue with steps 5 7 Otherwise unscrew the four thumbscrews h...

Page 270: ...ethod one wrench to hold the nebulizer fitting and the other to turn the compression fitting Figure 9 8 Removing the burner end cap 6 Optional Disconnect the drain tube and clamp if they are in place 7 Optional Unscrew the four knurled screws holding the end cap to the burner chamber and carefully remove the end cap 8 Remove the flow spoiler from inside the burner chamber ...

Page 271: ...seen under the burner chamber in 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 ...

Page 272: ... burner assembly 3 Place the flow spoiler 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 compr...

Page 273: ...ngs 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 3 Locate the drain vessel The drain tube and interlock cable will be attached to the drain vessel retainer cap 4 Place the drain vessel in full view on the floor in front of th...

Page 274: ...s 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 alignment You should readjust the burner any time the burner is cleaned or the burner head is replaced Installing AAnalyst Nebulizer Install the AAnalyst n...

Page 275: ... 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 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...

Page 276: ...e 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 Figure 9 10 The burner drain system ...

Page 277: ...ing 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 Figure 9 11 Replacing the drain tubing WARNING Dispose of drain vessel w...

Page 278: ...drain tubing Then attach the tubing to the drain outlet on the burner end cap Tighten the clamp securely 8 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 9 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 P...

Page 279: ... 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 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 ...

Page 280: ...is clean The burner is correctly optimized 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 to clean the capillary holder The first simplified way should be used if the nebulizer is not difficult to clear This method involves simply pa...

Page 281: ...cedure below Removal and Disassembly the Nebulizer 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 ...

Page 282: ... well Handle with care See the next page for instructions 6 Unscrew the capillary tubing Refer to 7 Figure 9 13 and loosen and then remove the adjustment nut P N N037 1492 and locking ring 8 Remove the capillary assembly from the nebulizer body Cleaning 1 While holding the capillary assembly in one hand take one of the cleaning wires P N 0303 0135 supplied 2 Push it through the capillary assembly ...

Page 283: ... 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 2 Then rotate it holding only the base approximately 1 8 turn clockwise i e until it reac...

Page 284: ...mended 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 clo...

Page 285: ... 6 While still aspirating the standard turn the nebulizer locking nut clockwise until it is free of the nebulizer adjustment nut 7 Slowly turn the nebulizer adjustment nut counter clockwise until bubbles begin to appear at the end of the capillary tube in the sample solution 8 Slowly turn the nebulizer adjustment nut clockwise until the absorbance goes to a maximum and then begins to decrease 9 Lo...

Page 286: ...mportant 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 nebuliz...

Page 287: ...tory detergent solution or a solvent such as isopropanol preferably in an ultrasonic bath 4 Rinse all the cleaned components thoroughly with deionized water 5 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 water If they look damaged replace them 6 After you...

Page 288: ... 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...

Page 289: ... 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 f...

Page 290: ...sh the flame if lit 2 From the front of the instrument swing open the compartment door and locate the E Box 3 Turn the power switch off and remove the AC power cord from the E Box 4 Disconnect power cord and all cables that are connected to the ports on the front of the E Box 5 Unscrew the door using an Allen wrench 6 Unscrew the flathead locking screw located below the printer connection port 7 U...

Page 291: ...AAnalyst 200 User s Guide 9 47 Figure 9 15 Removing the E Box from the instrument ...

Page 292: ...andles 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 7 Close the compartment door ...

Page 293: ...AAnalyst 200 User s Guide 9 49 Figure 9 16 Replacing the E Box ...

Page 294: ...larly 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 pr...

Page 295: ... emitted by these lamps can harm your eyes 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...

Page 296: ... Removing the Deuterium Lamp Assembly 1 Turn OFF the power switch and unplug the power cord from the E Box WARNING Wait a sufficient amount of time for the background corrector lamp to cool before replacing it 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...

Page 297: ...is will decrease the UV performance 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...

Page 298: ... screws of the deuterium lamp 1 Set up the standard conditions for copper including slit 2 Go to 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 T...

Page 299: ...AAnalyst 200 User s Guide 9 55 Figure 9 20 The centering of the two lamp beams The alignment procedure is now complete ...

Page 300: ...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...

Page 301: ... 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 Figure 9 21 Mounting the quartz cell holder onto the burner head rear view 2 Refer to the next figu...

Page 302: ...lder 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 WARNING 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 ...

Page 303: ...AAnalyst 200 User s Guide 9 59 Figure 9 23 Installing the quartz cell onto the holder 3 Carefully lower the cell holder bracket to the down position ...

Page 304: ...01 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 Standard 0990 2147 Organics Corkprene 0047 2014 O Ring Burner Cap Organics Kalrez 0992 1044 O ring for the burner head 0990 2219 Nebulizer and Components Descri...

Page 305: ...0160 Plug Adaptors for use of HCL Description PE Part Number Plug Adapter for use of coded Intensitron HCL N305 0196 Plug Adapter for use of non coded Intensitron HCL N305 0197 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 035...

Page 306: ...ries 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 ...

Page 307: ...Troubleshooting 10 ...

Page 308: ......

Page 309: ...lp 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 othe...

Page 310: ...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 Use a background corrector or if applicable use a nitrous oxide acetylene flame The sample matrix may be less viscous than the standards Remake the standards in the same matrix as the samples or use the method of add...

Page 311: ...using the correct wavelength Check the wavelength If a problem is found contact a PerkinElmer service engineer for assistance If the element is easily ionized ionization suppressant may be required Add approximately 1000 mg L of an easily ionized salt such as potassium lithium or lanthanum to samples standards and blank The fuel and oxidant flows may not be set properly or the wrong type of flame ...

Page 312: ...llel to the light beam The burner position may be incorrect Adjust the horizontal vertical and rotational position using the information in this User s Guide The instrument may have been autozeroed while a sample was being aspirated Autozero the instrument while aspirating a blank Cannot get suggested detection limits Characteristic concentration may not be within 20 of the standard conditions val...

Page 313: ...n the Maintenance chapter Check for proper drainage Noise may be due to a highly absorbing flame in far ultraviolet range Use background correction or vary the gas flows to minimize flame absorption or maximize flame stability Noise may be due to a weak lamp coupled with a highly absorbing flame increase the lamp current to the max rating replace the lamp use the next widest slit setting although ...

Page 314: ...r head must be used for all nitrous oxide acetylene analyses N20 C2H2 Check to make sure the correct burner head is installed fully seated and secured The drain interlock may not be connected Make sure the drain interlock connection has been made The level of liquid in the drain vessel may be too low Pour about 200 300 mL of deionized water into the neck of the burner or directly into the top of t...

Page 315: ... ones listed below Reignite the flame only after the problem has been corrected Contact a PerkinElmer service representative for assistance Fuel and oxidant gas lines may have been inadvertently switched Check the connections at the burner and at the gas supplies The burner system may leak Check the condition of all o rings burner head end cap o ring on nebulizer front end cap Replace o rings that...

Page 316: ...a flashback If a lean flame is required adjust the nebulizer uptake rate Gas connections may be loose or a leak may have occurred If you suspect a leak in the gas lines immediately close the cylinder valve If you need 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 bub...

Page 317: ...e if necessary Hollow cathode lamp will not light Instrument is off or not plugged in Turn instrument on or plug into line power Lamp not plugged in Connect lamp Lamp worn out or damaged Try another lamp Insufficient lamp current Set the proper current EDL Electrodeless Discharge Lamp will not light The lamp may not be connected to the EDL power supply Check the lamp cable plug it in if it is not ...

Page 318: ...he lamp current Use the recommended value listed on the lamp label The slit width may be too small Check the recommended settings for the element in the Recommended Conditions window The wrong wavelength for the element may be specified Refer to the Recommended Conditions window for the element ...

Page 319: ...ponents 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 Check and or Remedy Background source intensity is much lower than the primary source May not need to use the background corrector Det...

Page 320: ...Troubleshooting 10 14 ...

Page 321: ...Index ...

Page 322: ......

Page 323: ...yze samples page 7 22 7 24 atomic absorption 7 7 auto scale graph 7 24 button on flame page 7 13 auto zero graph button on Flame page 7 13 autosampler tray analyze samples page 7 26 autosampler maintenance 9 50 servicing 9 50 spare parts 9 50 autosamplers 9 53 calculated intercept analyte addition 7 19 acetylides safety 2 7 air compressor requirements 3 16 connecting 5 15 cylinder information 3 17...

Page 324: ...ycling 5 7 checklists general maintenance 9 8 chemicals safety 2 20 3 6 cleaning lamps 4 10 compressed gases 2 14 connection display 5 24 EDL 1 5 24 EDL 2 5 24 electrical supply 4 19 ethernet 5 24 foot switch 5 24 5 26 keyboard 5 24 power entry module 5 24 power switch 5 24 printer 5 24 serial 1 5 24 connection autosampler customer service 10 3 cyanide solutions safety 2 7 D deuterium arc backgrou...

Page 325: ...ing your lab 3 4 ethernet connection 5 24 exhaust capacity 3 13 vent 3 12 vent kit 3 14 explosion acetylene 3 18 extinguish flame 6 43 F figures after decimal 7 17 first sample location 7 26 flame emmision 7 7 flame on off button 7 13 flame page description 7 11 fittings acetylene supply 3 19 flame igniting 6 35 troubleshooting 10 8 flame atomization safe operation of the flame 2 10 safe use of bu...

Page 326: ... 7 maintenance 4 10 parameters 7 9 replace 4 10 9 45 removing 6 24 on off 7 9 troubleshooting 10 3 types used 4 6 7 9 uncoded lamp 6 30 7 10 M maintenance autosampler 9 50 burner chamber disassembling 9 25 burner install 9 26 checklist burner system 9 9 checklist general 9 4 checklist instrument 9 5 cleaning spills 9 4 cleaning instrument 9 6 drain system 9 29 drain system flushing 9 30 E Box remo...

Page 327: ...eplicates 7 21 analyze page 7 26 dialog in Spectrometer subpage replicates in Spectrometer subpage 7 16 entry on spectrometer subpage 7 16 requirements air 3 16 electrical 4 19 gas 3 15 laboratory 3 7 3 14 nitrous oxide 3 17 reslope dialog in Calibration subpage reslope in Calibration subpage 7 18 entry on calibration subpage 7 18 result window analyze page 7 25 sample page 7 21 rinsing the burner...

Page 328: ...tion zero 7 18 tools dialog description 7 27 touch screen 6 19 installation 5 10 user interface components 6 20 7 4 troubleshooting 10 3 burner problems 10 8 deuterium arc background corrector 10 13 flame analysis problems 10 4 flame problems 10 8 lamp problems 10 11 tubing acetylene supply 3 19 U units entry on Calibration subpage 7 17 unpacking spectrometer 5 4 user interface components dialogs ...

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