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Summary of Contents for Endress+Hauser analytikjena HS 55
- Page 1 Operating Manual HS 55 (Batch Mode) Hg/Hydride System HydrEA System...
- Page 2 Manufacturer Analytik Jena GmbH Konrad-Zuse-Strasse 1 07745 Jena / Germany Phone: +49 3641 77 70 Fax: +49 3641 77 9279 Email: info@analytik-jena.com Technical Service Analytik Jena GmbH Konrad-Zuse-Strasse 1 07745 Jena / Germany Phone: +49 3641 77 7407 Fax: +49 3641 77 9279 Email: service@analytik-jena.com For a proper and safe use of this product follow the instructions.
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Page 3: Table Of Contents
HS 55 (Batch Mode) Table of contents Table of contents 1 Basic information................................About this operating manual ........................... Intended use ..............................2 Security .................................... Safety labeling on the device ........................... Requirements for the operating personnel..................... Safety instructions – transport and installation....................Safety instructions –... - Page 4 Table of contents HS 55 (Batch Mode) Inspecting and replacing the flange seal in the batch module ..............41 Replacing the hose dryer..........................41 Replacing the gold collector..........................41 Maintaining the HydrEA system ........................42 6.8.1 Cleaning the coated graphite tube ........................42 6.8.2 Evaporating the iridium or gold coat.......................
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Page 5: Basic Information
HS 55 (Batch Mode) Basic information Basic information About this operating manual Content This operating manual describes the HS 55 Hg/hydride system. The device is intended to be operated by qualified specialist personnel observing the op- erating manual. The operating manual provides information about the design and operation of the de- vice and provides operating personnel the necessary know-how for the safe handling of the device and its components. -
Page 6: Intended Use
Basic information HS 55 (Batch Mode) Intended use The Hg/hydride system must 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. -
Page 7: Security
HS 55 (Batch Mode) Security Security For your own safety and to ensure error-free and safe operation of the device, please read this chapter carefully before commissioning. Observe all safety instructions listed in this user manual and all messages and infor- mation displayed on the monitor by the control and analysis software. -
Page 8: Requirements For The Operating Personnel
Security HS 55 (Batch Mode) Requirements for the operating personnel The device must only be operated by qualified specialist personnel instructed in the use of the device. This instruction also include teaching the contents of this user manual and of the user manuals of the connected system components. We recom- mend training by qualified employees of Analytik Jena or its representatives. -
Page 9: Safety Instructions - Protection Against Explosion And Fire
HS 55 (Batch Mode) Security Protective and safety equipment must never be removed, modified or switched ¡ off during operation. ¡ Free access to the power switch on the right side panel must be ensured during operation. Modifications, conversions and extensions to the device are only permitted after ¡... -
Page 10: Safety Instructions For The Operation Of Compressed Gas Containers And Compressed Gas Systems
Security HS 55 (Batch Mode) 2.4.3 Safety instructions for the operation of compressed gas containers and compressed gas systems ¡ The operating gases are taken from compressed gas containers or local com- pressed gas systems. The operating gases must have the required purity. Work on compressed gas containers and systems may only be carried out by indi- ¡... -
Page 11: Safety Instructions - Maintenance And Repair
HS 55 (Batch Mode) Security The only suitable cleaning method for the housing is wipe disinfection. If the dis- ¡ infectant has a spray nozzle, apply disinfectant to a suitable cloth before using it on the device. Particular care must be taken if infectious materials are analyzed with the device, as the device cannot be decontaminated as a single unit. -
Page 12: Function And Design
Function and design HS 55 (Batch Mode) Function and design Function and measuring principle Hydride method The hydride method enables the matrix-free detection of the elements As; Bi; Sb; Se; Sn; Te. It is based on the formation of gaseous metal hydrides through reduction of the acidic samples with sodium borohydride (NaBH ). -
Page 13: Design
HS 55 (Batch Mode) Function and design You can extend the functionality of the HS 55 and HS 60 Hg/hydride systems with the following accessories and modules: Module Function Hg cell ("tulip") Tulip-shaped cell for higher sensitivity for Hg detection Hg Plus Upgrade Modul Enrichment of mercury on a gold collector for ultra-trace analy- HydrEA Upgrade Kit... -
Page 14: Figure 2 Front View With Main Assemblies
Function and design HS 55 (Batch Mode) All functionally relevant assemblies are located on the front plate of the batch functional module: ¡ 1-channel hose pump for the reduction agent transport ¡ Batch module as reaction unit Push button to start the measuring process ¡... -
Page 15: Hose Pump
HS 55 (Batch Mode) Function and design Remove the reaction beaker after the measuring process, rinse it and refill it with sam- ple. 1-channel hose pump Purge gas Transport gas Gas outlet Drying hose 4-valve group Reaction beaker Solenoid Reduction agent valve Cell Gold collector... -
Page 16: 4-Valve Group For Gas Control
Function and design HS 55 (Batch Mode) Figure 4 Batch module 1 "purge gas" gas supply 2 "transp. gas" gas supply 3 Metering hose for reduction agent 4 "to cell" gas outlet 5 Head 6 Reaction beaker Reduction agent and purge gas are transported through the metering tip to the bottom of the reaction beaker. -
Page 17: Hg Plus Upgrade Modul (Optional)
HS 55 (Batch Mode) Function and design 3.2.4 Hg Plus Upgrade Modul (optional) The optional module is located in a compartment at the top of the Hg/hydride system. You can open the red cover of the Hg/hydride system and access the module. The module consists of the following components: quartz tube with the gold collector ¡... -
Page 18: Type Plate
Function and design HS 55 (Batch Mode) 3.2.5 Type plate The type plate is located on the rear of the device. The type plate contains the following information: ¡ company name and complete address of the manufacturer ¡ device designation: type designation and trade name ¡... -
Page 19: Figure 6 Graphical Display: Gas Paths And Measuring Process
HS 55 (Batch Mode) Function and design Plot Parameters Graphic for Take up sample Pump time Take up reductant first measurement Take up wash sol. Sample valve to reactor Reagent transport Autozero Gas paths and flows Delay time Measurement React. Coll. -
Page 20: Installation And Commissioning
Installation and commissioning HS 55 (Batch Mode) Installation and commissioning Normally, the Hg/hydride system is installed by the Analytik Jena customer service or persons authorized by Analytik Jena together with the AAS device. If the Hg/hydride sys- tem is delivered separately at a later time, you can also install it yourself. When installing and commissioning the system, observe the information in the "Safety instructions"... -
Page 21: Figure 7 Quartz Cell For Hydride Method
HS 55 (Batch Mode) Installation and commissioning } Fold the cell unit upwards. Insert a suitable cell: Figure 7 Quartz cell for hydride method Figure 8 Hg cell (made of quartz, tulip-shaped) } For the hydride method: Insert the quartz cell. } Close and lock the cell unit. } Attach the frames with the quartz windows on both sides and clamp them in place with the leaf springs. -
Page 22: Figure 9 Cell Unit With Quartz Cell
Installation and commissioning HS 55 (Batch Mode) Figure 9 Cell unit with quartz cell 1 Quartz cell for hydride method 2 Frame with quartz window 3 Lock Installing the cell unit on the ZEEnit 650 P The ZEEnit 650 P model is only equipped with a graphite tube furnace. In this model, the graphite tube furnace can be pulled out of the sample chamber and the cell unit for the Hg/hydride method can be installed. -
Page 23: Installing The Hg/Hydride System On The Aas
HS 55 (Batch Mode) Installation and commissioning Figure 11Receptacle and cell unit for Hg/hydride system 1 Receptacle for cell unit 2 Attachment screw 3 Cell unit } Insert the corresponding cell into the cell unit and proceed as described at the begin- ning of this chapter. -
Page 24: Figure 12 Hg/Hydride System Installed On The Aas
Installation and commissioning HS 55 (Batch Mode) Figure 12Hg/hydride system installed on the AAS } Place the Hg/hydride system to the right of the AAS device or onto a table next to the AAS device. Electrical connection and inter- } Connect the cell unit electrically to the Hg/hydride system: faces –... -
Page 25: Figure 13 Connections On The Right Of The Device
HS 55 (Batch Mode) Installation and commissioning Figure 13Connections on the right of the device 1 Cell unit temperature sensor connection 1a Knurled screw for grounding ("cell sensor") 2 Connection for +5 V/+24 V supply from 3 "AAS/RS 232" interface the AAS 4 Argon connection 5 "cell heating"... -
Page 26: Figure 14 Hose Routing For The "Hydride"/"Hg Without Enrichment" Mode
Installation and commissioning HS 55 (Batch Mode) Figure 14Hose 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 batch module via the connection hose. -
Page 27: Changing Between Operating Modes
HS 55 (Batch Mode) Installation and commissioning } Switch on the Hg/hydride system. } Switch on the AAS device. ü First measurements can be started. 4.1.3 Changing between operating modes To change between the "Hydride" or "Hg without enrichment" and "Hg with enrichment" modes, you have to change the hose routing on the front plate of the batch module. -
Page 28: Retrofitting The Hg Plus Upgrade Modul
Installation and commissioning HS 55 (Batch Mode) Figure 17Hose routing for the "Hg with enrichment" mode Selecting the cell } "Hydride" mode: use the quartz cell. } Insert the cell into the cell unit of the AAS device and close it with the quartz win- dows. - Page 29 HS 55 (Batch Mode) Installation and commissioning } Open the red hood of the Hg/hydride system. } Pull the short-circuit plug in the Hg/hydride system up and remove it. } Insert the module. To do so, align the module with the guide pins and push it down until the plug-in connection has been established.
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Page 30: Installing The Hydrea System
Installation and commissioning HS 55 (Batch Mode) } Close the Hydride system window. ü The new module is ready for operation. Installing the HydrEA system NOTICE Error message when the dummy plug is missing No cell unit is used for the HydrEA method. The Hg/hydride system emits an acoustic signal if the temperature sensor connection is open. -
Page 31: Coating The Graphite Tube
HS 55 (Batch Mode) Installation and commissioning } For AAS devices with only one sample chamber: remove the cell and also remove the cell unit. 4.3.2 Coating the graphite tube NOTICE Damage to the titanium cannula Do not coat the graphite tube using the titanium cannula of the autosampler for the graphite tube furnace. -
Page 32: Installing The Hg/Hydride System On The Aas
Installation and commissioning HS 55 (Batch Mode) Ir coating program Step Temperature Rate [°C/s] Hold time [s] Purge gas [°C] Drying Drying Drying Pyrolysis 1200 Stop Atomizing 2100 Stop Bake-out 2100 Medium Au coating program Step Temperature Rate [°C/s] Hold time [s] Purge gas [°C] Drying... -
Page 33: Figure 18 Connections On The Right Of The Device
HS 55 (Batch Mode) Installation and commissioning Figure 18Connections on the right of the device 1 Cell unit temperature sensor connection 1a Knurled screw for grounding ("cell sensor") 2 Connection for +5 V/+24 V supply from 3 "AAS/RS 232" interface the AAS 4 Argon connection 5 "cell heating"... -
Page 34: Adjusting The Autosampler For The Graphite Tube Furnace With The Titanium Cannula
Installation and commissioning HS 55 (Batch Mode) This leads to the following activation sequence: } Switch on the Hg/hydride system. } Switch on the AAS device. ü First measurements can be started. 4.3.4 Adjusting the autosampler for the graphite tube furnace with the titanium cannula } Start the ASpect LS or ASpect CS program. -
Page 35: Operation
HS 55 (Batch Mode) Operation Operation How to prepare the AAS device for the hydride or HydrEA method is described in the user manual for the AAS device. The software manual describes the following: ¡ how to set the method and the operating mode ¡... - Page 36 Operation HS 55 (Batch Mode) If possible, treat standards and samples identically. When arsenic standards age, ¡ As(+V) ions form in the solution due to reaction with atmospheric oxygen. Suggestion for preparing the solutions Reduction agent Solution Preparation Shelf life, comments Master solution Dissolve 7.5 g NaBH Approx.
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Page 37: Switching The Device On And Off
HS 55 (Batch Mode) Operation Solution Preparation Shelf life, comments Standards Example: 1 µg/l As standard Prepare the standards fresh on a daily basis. 0 / 0.2 / 0.4 / 0.6 / 0.8 / 1 ml of solution 3 + 1.0 µg/l As 7 ml HCl (37 %, p. a.) + 1 ml KI/ascorbic acid solu- tion After 45 minutes, fill up with... -
Page 38: Maintenance And Care
Maintenance and care HS 55 (Batch Mode) Maintenance and care The operator may not undertake any service or maintenance work to this device and its components other than that specified in these instructions. Observe the information in the "Safety instructions" section for all maintenance work. Compliance with the safety instructions is a prerequisite for the error-free operation of the device. -
Page 39: Cleaning The Cell And The Cell Windows
HS 55 (Batch Mode) Maintenance and care Cleaning the cell and the cell windows Clean the cell and the cell windows when the measured lamp energy, i.e., the number of counts, drops. In devices with a Zeeman furnace, contamination can be detected by an increase in the PMT voltage. -
Page 40: Inspecting And Replacing The Pump Hose
Maintenance and care HS 55 (Batch Mode) } Then flush the cell windows with distilled water and allow them to dry without any residues, e.g., by purging them with an inert gas. ü The cell windows have been cleaned. Cleaning the cell } After the cell unit has cooled down: unlock and unfold the cell unit. -
Page 41: Inspecting And Replacing The Flange Seal In The Batch Module
HS 55 (Batch Mode) Maintenance and care Inspecting and replacing the flange seal in the batch module After an extended operating time, the sealing ring at the head of the batch module may lose its elasticity and sealing effect and must be replaced. } Turn the reaction beaker and pull it off the flange. -
Page 42: Maintaining The Hydrea System
Maintenance and care HS 55 (Batch Mode) Figure 19Gold collector 1 Gas inlet 2 Heating wire 3 Gas outlet 4 Heating connection 5 Infrared sensor 6 Heating connection } Unscrew the gas inlet and gas outlet hoses from the gold collector. } Pull the heating coil connections off the PCB. -
Page 43: Evaporating The Iridium Or Gold Coat
HS 55 (Batch Mode) Maintenance and care } In the Quick Start window, select the HydrEA method and initialize the device config- uration. } Close the window with OK. } Click the Furnace button. } Select the Control tab and enter the parameters for cleaning the graphite tube in the Clean furnace area: –... -
Page 44: Troubleshooting
Troubleshooting HS 55 (Batch Mode) Troubleshooting Strong foaming can occur in the sample during the hydride and Hg cold vapor meth- ods. Test the foaming of unknown samples. ¡ Immediately stop the measuring process if the transport gas argon transports ¡... -
Page 45: Transport And Storage
HS 55 (Batch Mode) Transport and storage Transport and storage Transport When transporting the device, observe the safety instructions in the "Safety instructions" section. Avoid the following during transport: Impact and vibration ¡ Risk of damage due to shock, impact or vibration! ¡... -
Page 46: Moving The Device In The Laboratory
Transport and storage HS 55 (Batch Mode) } Remove the cell from the cell unit. } Remove the cell unit. } Empty and rinse out the storage bottle. } Turn the reaction beaker to remove it from the batch module. } Pack open hose ends in protective bags and attach them to the device, e.g., with ad- hesive tape. -
Page 47: Storage
HS 55 (Batch Mode) Transport and storage Storage NOTICE Risk of device damage due to environmental conditions Environmental influences and condensation can destroy individual components of the device. ¡ Only store the device 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. -
Page 48: Disposal
Disposal HS 55 (Batch Mode) Disposal Auxiliary and operating materials as well as their containers may not be disposed of as domestic waste or enter the sewage system or the soil. The residual liquid 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. -
Page 49: Specifications
HS 55 (Batch Mode) Specifications Specifications 10.1 Technical data General characteristics Designation/type HS 55 Dimensions (W x H x D) 360 x 370 x 240 mm Mass 14 kg Procedural data Mode Batch mode (discontinuous) Detectable elements As; Bi; Hg; Sb; Se; Sn; Te Methods ¡ Hydride method Hg cold vapor method without enrich- ¡... -
Page 50: 10.2 Standards And Directives
Specifications HS 55 (Batch Mode) Gas flow Purge gas: 15 l/h ¡ Transport gas: 6 l/h, 25 l/h, 31 l/h ¡ Electrical variables Voltage Depending on the basic module: 220 to 230 V or 100 to 110 V Frequency 50/60 Hz Fuses G-fuse sets (5 x 20 mm) F1/F2 ¡ T 3.15 A H for 220 to 230 V ¡ T 6.3 A H for 100 to 110 V Power consumption (during heating) 650 VA... -
Page 51: Revision Overview
HS 55 (Batch Mode) Revision overview Revision overview Version Effective date Changes 2019-09 First version Note: New version labeling after introduction of the Document Management System (A, B, etc.) 2021-01 Change of the company' s legal form 2021-11 ¡ Installation on current AAS device models ¡... - Page 52 Table of figures HS 55 (Batch Mode) Table of figures Figure 1 Hg/hydride system with AAS device ....................... 13 Figure 2 Front view with main assemblies........................14 Figure 3 Functional diagram ............................15 Figure 4 Batch module ..............................16 Figure 5 Gold collector..............................
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