Endress+Hauser analytikjena HS 55, Operating Manual

Page 1: ...Operating Manual HS 55 Batch Mode Hg Hydride System HydrEA System ...

Page 2: ...Strasse 1 07745 Jena Germany Phone 49 3641 77 7407 Fax 49 3641 77 9279 Email service analytik jena com General Information http www analytik jena com Documentation Number 10 1700 002 23 Edition C 11 2021 Technical Documentation Analytik Jena GmbH Copyright 2021 Analytik Jena GmbH For a proper and safe use of this product follow the instructions Keep the operating manual for future reference ...

Page 3: ...15 3 2 2 Batch module 15 3 2 3 4 valve group for gas control 16 3 2 4 Hg Plus Upgrade Modul optional 17 3 2 5 Type plate 18 3 3 Measuring process 18 4 Installation and commissioning 20 4 1 Installing the hydride and Hg cold vapor systems 20 4 1 1 Installing the cell unit 20 4 1 2 Installing the Hg hydride system on the AAS 23 4 1 3 Changing between operating modes 27 4 2 Retrofitting the Hg Plus U...

Page 4: ...8 1 Cleaning the coated graphite tube 42 6 8 2 Evaporating the iridium or gold coat 43 7 Troubleshooting 44 8 Transport and storage 45 8 1 Transport 45 8 1 1 Preparing the device for transport 45 8 1 2 Moving the device in the laboratory 46 8 1 3 Returning the device for servicing 46 8 2 Storage 47 9 Disposal 48 10 Specifications 49 10 1 Technical data 49 10 2 Standards and directives 50 11 Revisi...

Page 5: ...e numbered and combined into action units Warnings are indicated by a warning triangle and a signal word The type source and consequences of the hazard are stated together with notes on preventing the hazard Elements of the control and analysis program are indicated as follows Program terms are in bold e g the System menu Buttons are indicated by square brackets e g OK Menu items are separated by ...

Page 6: ...st only be used in connection with an atomic absorption spectrometer by Analytik Jena The device and its components may only be used for the analyses listed in the user man ual Only this specified use is regarded as the intended use ensuring the safety of the user and the device ...

Page 7: ... ard location On the cell heating connection dan gerous electrical voltage warning Only connect and disconnect the connec tion cable when the device is switched off Warning about hot sur face On the red device hood there is a risk of burns on the Hg Plus Upgrade Modul optional Allow the module to cool down before opening the hood Caution Hot warn ing sign Warning about hot sur face On the cell hea...

Page 8: ... device grip the device firmly at the bottom with both hands and lift it Ensure that the device is completely empty Flush the pump and metering hoses thoroughly to prevent reduction agent solution from dripping out The solution is corrosive and harmful to health and damages clothing Remove the storage bottle for reduction agent Empty the bottle before trans port Insufficiently secured components p...

Page 9: ...e caught in the pump and drawn in Wear suitable hair protections and tight fitting clothing 2 4 1 Safety instructions protection against explosion and fire The device may not be operated in an explosive environment Smoking or handling open flames are prohibited in the room in which the device is operated 2 4 2 Safety instructions electrical equipment Lethal voltages may occur in the device Contact...

Page 10: ... in the safety data sheets from the manufacturers of the auxiliary and op erating materials must be complied with Only operate the device when the exhaust unit is active Ensure good room ven tilation in working rooms Cleaning with hydrofluoric acid must be carried out in an exhaust chamber The operator must wear a rubber apron gloves and a face mask when handling hy drofluoric acid When measuring ...

Page 11: ...ance and care chapter may be per formed by the operator Only clean the exterior of the device with a slightly moistened non dripping cloth Use only water and if required customary surfactants All maintenance and repair work on the device must only be carried out when the device is switched off unless specified otherwise The gas supply must be shut off before performing any maintenance or repair wo...

Page 12: ...the hydride form ing elements As Bi Sb Se Sn Te or Hg with the graphite tube furnace The Hg hydride system generates the gaseous metal hydrides or the atomic Hg vapor respectively The autosampler for the graphite tube furnace AS GF transfers the ana lytes with the carrier gas argon into the graphite tube furnace There the metal hydrides are enriched on the iridium coated standard tube for wall ato...

Page 13: ...les to the AAS You can retrofit these accessories and modules yourself 3 2 Design The Hg hydride system consists of a basic module the functional module and an op tional module for mercury enrichment The three modules are plugged on top of each other and electrically connected through mixed plug connectors The Hg hydride system can be used with the following AAS devices ZEEnit 700 P ZEEnit 700 Q Z...

Page 14: ...m above and electrically connected to it The hoses are routed to the frame of the func tional module and from there to the front plate When changing between the Hydride batch Hg without enrichment batch and Hg with enrichment batch modes you only change the hose routing on the front plate Supply the sample manually into the Hg hydride system To do so pipette a volume of 1 to 20 ml into the reactio...

Page 15: ...nance work Renew all hoses that have come into contact with the reduction agent Flush the Hg hydride system thoroughly before loading samples the next time 3 2 1 Hose pump The 1 channel hose pump is equipped with an adjustable snap in cartridge and an Ismaprene pump hose with an inner diameter of 2 06 mm The pump only runs during the pump time and transports reduction agent in 4 selectable speed s...

Page 16: ...tion The transport gas transp gas enters the reaction beaker at the top The transport gas transports the metal hydride or the Hg vapor from the reaction beaker to the atomizer in the AAS device or to the gold collector 3 2 3 4 valve group for gas control The 4 valve group provides fixed gas flows controlled by the software Valve MV2 Gas flow F2 with a flow of 15 l h Constant purge gas flow through...

Page 17: ...ule It contains a loosely rolled up gold plat inum mesh which is approx 20 mm wide The mesh is secured in the quartz tube The gold collector enriches the mercury from the reaction gas on its surface by means of amalgamation Mercury is only released again from the gold collector when heated to a temperature of approx 630 C during bake out The quartz tube is surrounded by a heating coil The heating ...

Page 18: ...ue is determined over a period of 2 s instead of 4 s Measuring process with enrich ment Before a sample is supplied to the atomizer of the AAS device the Hg hydride system enriches mercury from one or more samples on the gold collector The gold collector re leases the mercury again during bake out With the subsequent cooling the Hg hydride system prepares the gold collector for the next measuremen...

Page 19: ...le pump Sample valve Reagents Measurement Collector Time s Take up sample Take up reductant Take up wash sol Sample valve to reactor Reagent transport Autozero Delay time Measurement Heat collector Cool collector AZ Wash 2 Close Gas paths and flows Line 6 Pump time Figure 6 Graphical display gas paths and measuring process ...

Page 20: ... the hydride and Hg cold vapor systems NOTICE Continuous beeping tone in the case of incomplete installation If the installation is incomplete the device emits a continuous beeping tone In this case review the installation steps carried out Information on the AAS device can be found in the separate operating manual 4 1 1 Installing the cell unit WARNING Risk of oxyhydrogen formation The cell must ...

Page 21: ... of the cell The gas hose connection on the Hg hydride system is marked to cell Also attach the gas discharge hose to the outer connections If possible hook the T piece into the sample chamber panel at the rear of the sample chamber Route the gas discharge hose into the extractor For the Hg cold vapor method Insert the Hg cell Close and lock the cell unit Secure the Hg cell with the tension spring...

Page 22: ...d out of the sample chamber and the cell unit for the Hg hydride method can be installed Unscrew the attachment screw on the front under the graphite tube furnace Pull the graphite tube furnace out of the sample chamber Lock the furnace plate in the pulled out position with the locking pin Figure 10Locking pin on the furnace plate Insert the receptacle for the cell unit into the corresponding sock...

Page 23: ... of this chapter 4 1 2 Installing the Hg hydride system on the AAS CAUTION Dangerous voltage at the cell heating connection Dangerous voltage may be present at the cell heating connection Only connect the device and the other components to the power grid when they are switched off Only connect and disconnect electrical connection cables between the system com ponents when the system is switched of...

Page 24: ... sensor cable on the connection panel of the Hg hy dride system with the knurled head screw Connect the functional module to the AAS the AAS device provides the voltages 5 V 24 V for the functional module Connect the AAS plug of the twin cable to the AS or Sampler Flame socket on the AAS device Connect the HS D sub socket of the thinner cable of the twin cable to the input 5 V 24 V connection of t...

Page 25: ...ule Connect the power cable to the power connection on the basic module Use the mul tiple socket provided with the AAS device for the connection Connect the Argon hose to the bulkhead fitting on the rear Hydride Hg without enrich ment mode Select the drying hose Hy for the hydride method or Hg for mercury detection Connect the cell hose to the drying hose via the female Luer coupling Connect the d...

Page 26: ...the storage bottle with the reduction agent Connect the reduction agent intake hose with the blue hollow screw to the pump hose of the 1 channel pump and immerse it into the storage bottle for the reduction agent up to the stopper Hook the hose cartridge into the Hg hydride system Set the locking levers so that the solution is transported evenly ü The Hg hydride system is now installed on the AAS ...

Page 27: ...ying hose via the female Luer coupling Connect the drying hose via the connection hose to the to cell gas outlet of the batch module If not already done attach the cell hose to the middle connection of the cell Figure 16Hose routing for the Hydride Hg without enrichment mode Hg with enrichment mode Select the drying hose type Hg Connect the drying hose to the gas connection marked to cell on the b...

Page 28: ...pgrade Modul WARNING Risk of electric shock There is a risk of touching live components and suffering an electric shock when con verting the Hg hydride system Before the conversion switch off the Hg hydride system and the AAS at the power switch Disconnect the power plug from the socket Disconnect all connection cables to the AAS and the cell unit Software tool for the conver sion Insert the CD in...

Page 29: ...ont connection with the black arrow 3 Close the red hood Connect the system to the power line the AAS device and the cell unit Switch on the devices first the Hg hydride system then the AAS After the devices have been initialized in the HS Wizard program click the Next button Exit the program Functional test Start the ASpect LS or ASpect CS program In the Quick Start window select the Hydride meth...

Page 30: ...th the titanium cannula for the HydrEA system 4 3 1 Preparing the analysis system for the HydrEA system CAUTION Dangerous voltage at the cell heating connection Dangerous voltage may be present at the cell heating connection Only connect the device and the other components to the power grid when they are switched off Only connect and disconnect electrical connection cables between the system com p...

Page 31: ...lic iridium or gold remains on the tube bottom Do not exceed a temperature of 2200 C iridium or 1000 C gold during coating and bake out of the graphite tube Otherwise iridium or gold loss will occur Start the ASpect LS or ASpect CS program In the Quick Start window select the Graphite Furnace Wall method and initialize the device configuration Close the window with OK Click the Furnace button Sele...

Page 32: ...nium cannula for the HydrEA system into the hose guide up to the bend and secure it Place the Hg hydride system near the AAS Electrical connection and inter faces On the Hg hydride system connect the dummy plug to the cell unit temperature sensor connection NOTICE Without the dummy plug the device emits a an acoustic signal Connect the functional module to the AAS the AAS device provides the volta...

Page 33: ...le and plug it onto the titanium cannula of the AS GF Reduction agent transport Fill the storage bottle with the reduction agent Connect the reduction agent intake hose with the blue hollow screw to the pump hose of the 1 channel pump and immerse it into the storage bottle for the reduction agent up to the stopper Hook the hose cartridge into the Hg hydride system Set the locking levers so that th...

Page 34: ...tructions Use the left right buttons to align the autosampler in the X direction parallel to the optical axis with the crosshair or the dosing opening Use the adjusting screws on the sides for fine adjustment Turn the adjusting screw to perform the adjustment in the Y direction sample chamber depth Tighten the screws and secure the setting with lock nuts Use the software to set the Z direction Low...

Page 35: ...id or lye WARNING Risk of poisoning due to arsenic The arsenic standard solution 1000 mg l causes severe skin and eye irritation The so lution is carcinogenic Wear protective goggles and protective clothing when handling this hazardous sub stance Observe all instructions and specifications in the safety data sheets When preparing diluted acids always fill in water first and slowly stir in the conc...

Page 36: ...ndard solution 1000 mg l As See manufacturer specifica tions Solution 2 1 mg l As 100 µl of solution 1 7 ml HCl 37 p a Fill up with H2O dist to 100 ml Stable for several days Prepare standards by means of a dilution series Standards 0 2 0 4 0 6 0 8 0 10 0 µg l As Example 10 µg l As stan dard 1 ml of solution 2 7 ml HCl 37 p a 1 ml KI ascorbic acid solu tion After 45 minutes fill up with H2O dist t...

Page 37: ...with reduction agent Start the control and analysis software In the Quick Start window select the Hydride method and initialize the device configuration Close the window with OK Click the Hydride syst button Select the Control tab and click the Load system button ü The device is ready for operation Tasks prior to daily shutdown Before closing the program asks you whether you would like to clean th...

Page 38: ...deformation If necessary replace the hoses As necessary and when the analytical perfor mance drops Clean the cell and the cell windows Replace the hose dryer Replace the gold collector Hg Plus Upgrade Modul Clean the coated graphite tube or evaporate the metal coat HydrEA Upgrade Kit and re coat the tube Replace the device fuses When changing the re duction agent Renew all hoses that have come int...

Page 39: ... explode at high temperatures would form in the cell Inspect the polished end faces of the cell Even if you notice only minor damage replace the cell CAUTION Risk of burns The cell is very hot directly after operation 600 to 950 C metal hydrides and 150 C mercury Allow the cell unit to cool down before maintenance Check the current cell temperature in the Hydride syst window on the Control tab NOT...

Page 40: ...hemical burns due to basic solution The hoses contain the basic reduction agent solution Prior to any maintenance work close the software and clean the system as sug gested The Hg hydride system flushes the hoses and pumps them out after re moval from the flushing solution Regularly inspect the pump and metering hoses for the reduction agent visually for wear stubborn contamination and deformation...

Page 41: ... to cell of the batch module and from the cell hose or the inlet marked to enr on the front plate Connect the new drying hose to the hose section at the outlet marked to cell of the batch module and the cell hose In the Hg with enrichment operating mode screw the second hose end with the hollow screw to the connection marked to enr on the front plate ü The new drying hose is ready for operation 6 ...

Page 42: ...neously insert the isolation sleeves on the heating wire into the groove Slide the gold collector up to the stop and screw it tight Plug the connections of the new heating coil onto the PCB Tighten the gas hoses on the right and left side of the gold collector with hollow screws ü The new gold collector is ready for operation 6 8 Maintaining the HydrEA system 6 8 1 Cleaning the coated graphite tub...

Page 43: ...00 C Au Attention The graphite material of the furnace starts to decompose at temperatures of 2600 C or higher You can then re coat the graphite tube from which the metal coat has been removed for the HydrEA system You can also use the graphite tube as a standard graphite tube for solution analysis standard operation Start the ASpect LS or ASpect CS program In the Quick Start window select the Hyd...

Page 44: ... hydride and Hg cold vapor meth ods Test the foaming of unknown samples Immediately stop the measuring process if the transport gas argon transports foam up to the quartz cell Add a few drops of anti foaming agent to strongly foaming samples e g Dow Corning DB 110A silicone anti foaming agent or octanol ...

Page 45: ... contains sodium borohydride and sodium hydroxide and is corrosive Wear protective goggles and protective clothing when handling the corrosive solu tion Observe all instructions and specifications in the safety data sheets Neutralize the basic solution and dispose of it professionally Also be careful when handling hoses They can contain residues of the corrosive so lution Exit the control and anal...

Page 46: ...device As the device does not have carrying handles grip the device firmly with both hands at the lower end Observe the guide values and adhere to the legally mandated limits for lifting and carrying loads without auxiliary means Observe the installation conditions at the new location 8 1 3 Returning the device for servicing Clean all device components from biologically hazardous chemical and radi...

Page 47: ...evice in air conditioned rooms Ensure that the atmosphere is free of dust and corrosive vapors If the device is not installed immediately after delivery or not required for longer periods it should be stored in its original packaging A suitable desiccant should be added to the equipment to prevent damage from moisture The requirements for the climatic conditions of the storage location can be foun...

Page 48: ...iquid from the Hg hydride system and the autosampler must be collected in the resistant 10 L bottle included in the scope of delivery of the AAS device The applicable regulations for the disposal of the residual substances must be observed At the end of its service life the device and its electronic components must be dis posed of as electronic waste in accordance with the applicable regulations ...

Page 49: ...ic temperature consistency 10 C Temperature for hydride forming elements 600 to 950 C Temperature for Hg room temperature or 150 C Absorption cells Quartz cells with removable quartz windows length 140 mm ID 15 mm Hg cell optional length 200 mm 1 channel hose pump Reduction agent transport Ismaprene hose ID 2 06 mm pump speed adjustable in 4 stages Reaction unit Batch module PTFE beaker with conic...

Page 50: ... category II EMC compatibility The device has been tested for radio interference elimination and interference immunity and fulfills the requirements of EN 61326 1 EU directives The device meets the requirements of the directive 2011 65 EU The device is designed and tested in accordance with standards meeting the require ments of EU directives 2014 35 EU and 2014 30 EU The device leaves the factory...

Page 51: ...ate Changes A 2019 09 First version Note New version labeling after introduction of the Document Management System A B etc B 2021 01 Change of the company s legal form C 2021 11 Installation on current AAS device models Inclusion of the document in the content manage ment system ...

Page 52: ...Figure 9 Cell unit with quartz cell 22 Figure 10 Locking pin on the furnace plate 22 Figure 11 Receptacle and cell unit for Hg hydride system 23 Figure 12 Hg hydride system installed on the AAS 24 Figure 13 Connections on the right of the device 25 Figure 14 Hose routing for the Hydride Hg without enrichment mode 26 Figure 15 Hose routing for the Hg with enrichment mode 26 Figure 16 Hose routing f...