HIGH TEMPERATURE REACTION CHAMBER
Contents
1. WAD U43 UV Quartz Window for the Vacuum Low Pressure DOMES WAD U23 Si Window for the Vacuum Low Pressure DOMES WED U23 CaF2 Window for the Vacuum Low Pressure DOMES WFD U23 ZnS Window for the Vacuum Low Pressure DOMES WID U23 ZnSe Window for the Vacuum Low Pressure DOMES WMD U23 KBr Window for the Vacuum Low Pressure DOMES WPD U23 Cooling Cartridge 2 HVC COL Purge Shield DRP PDR REPLACEMENT PARTS Overflow tray 11 0 116 989 Packing 116 836 Screen Set two each of three mesh sizes 4 7 mm 116 990 Screen Set 150 x 150 mesh 6 4 7 mm dia sss 116 990 1S Screen Set 250 250 mesh 6 4 7 mm dia sss 116 990 2S Screen Set 400 x 400 mesh 6 4 7 mm dia sse 116 990 3S K Type ThetrmocoOUple 2 i keen 008 144 Flex Mounting Plugs Male 008 266 1 00 x0 25 Cartridge Heater 100W 24V HTRS 26 24V Heater Assembly 5c ee e e eder HVC HT4 O Ring 10 for the VCO2. CARTRIDGE e Use a 1 16 hex head driver to clamp the cooling cartridge in place as shown using the clamp and screw provided TC Clamp TC Clamping Cooing Screw Cartridge Figure 8 Installing the Cooling Cartridge e Install the HVC in the Praying Mantis and install it into the spectrometer e Connect ID tubing from the barbed fittings to the chiller or recirculator Barbed Fittings 2 Figure 9 Cooling Cartridge Installed NOTE There is a temperature differential between the set temperature of the chiller or recirculator and the sample cup due to thermal losses through the tubes etc Use the HVC thermocouple to monitor this differential and fine tune the set temperature as needed 11 of 16 OPTIONS ABOUT THE PURGE SHIELD This optional purge shield slips into the Praying Mantis to improve the purge sealing around the front of the HVC INSTALLATION e Unscrew the thumbscrew on the top plate of the Praying Mantis e Carefully swing the top plate of the Praying Mantis out of the way e f the sampling stage or HVC is installed in the Praying Mantis unscrew the mounting screw and remove the sampling stage e Slide the purge shield into the Praying Mantis directly behind the front of the accessory as shown in Figure 10 e Push the purge shield slider up to allow room for installation of the HVC Purge Shield Slider Purge Shield Figure 10 Removing the Heating Cart
3. Fittings Viton 2 ORV 010 O Ring 10 for the VCO Fittings Kalrez sss ORK 010 O Ring 16 for the Bottom Cover Viton sss ORV 016 O Ring 16 for the Bottom Cover Kalrez ORK 016 O Ring 23 for the Dome ORV 023 O Ring 23 for the Dome Kalrez ssssssseeee emen ORK 023 O Ring 13 for Windows of the Dome Viton sse ORV 013 O Ring 13 for Windows of the Dome Kalrez ORK 013 PTFE Washer for the Windows 11 nnnm 116 429 UV Quartz Window for the Vacuum Low Pressure DOMES WAD U23 UV Quartz Window for the HVC DRP High Pressure Dome WAD U43 KBr Window for the Vacuum Low Pressure DOMES WPD U23 16 of 16 4 P SARRICK Manual Part No 09 n 2013 Harrick Scientific Products Inc
4. HARRICK gt GENERAL INFORMATION UNPACKING Before installing the High Temperature Reaction Chamber make sure all the parts on the included check list are present If any parts are missing or damaged contact Harrick Scientific immediately TECHNICAL SUPPORT For additional information please contact our Technical Support Center at 800 248 3847 between 9 a m and 5 p m EST or e mail your questions to techsupport harricksci com FEEDBACK Your comments and suggestions are welcome Please send them to Harrick Scientific Products Inc PO Box 277 141 Tompkins Ave 2 floor Pleasantville NY 10570 Phone 800 248 3847 Fax 914 747 7209 E mail info harricksci com Web www harricksci com 1 of 16 P d HARRICK gt ABOUT THE HVC ABOUT THE HIGH TEMPERATURE REACTION CHAMBER HVC The HVC is designed for operation up to 910 C under vacuum the lifetime of the heater is significantly reduced at temperatures above 450 C The pressure range is from high vacuum to pressures up to 3 44MPa or 25 8 ktorr the high pressure dome is required for pressures above 133 Pa or 1 ktorr At higher pressures the maximum operating temperature may be lower The HVC is made of chemically resistant 316 stainless steel Within the chamber is a temperature controlled sample stage with integral sample cup This stage incorporates a cartridge heater and a thermocouple It is thermally isolated from the outer chamber wall A water cooling jacket contro
5. reveal three access holes e Gingerly wipe or blow clean air through these holes to clean the interior of the HVC e When the interior is clean make sure the o rings on the bottom plate are clean and free of dirt e Re install the bottom cover The o rings used by the HVC should be replaced periodically HVC has o rings for sealing the windows o rings for sealing the access holes o rings on the fittings and an o ring to seal the dome to the HVC 14 of 16 4 TAARBRHICGK gt REPLACING THE HEATER AND OR THERMOCOUPLE Clamping Screw Ny Figure 12 Removing the Heating Cartridge and or HVC MAINTENANCE To replace the HVC heater Remove the HVC from the Praying Mantis if it is installed Use a 3 32 ball driver to unscrew the screw in the mounting block on the side of the HVC and remove the mounting block Use a slotted screwdriver to remove the screw and clamp on the back of the HVC that anchors the heater and thermocouple wire to the HVC Grasp the heater wires firmly and slide the heater out If replacing the thermocouple slide the old thermocouple out of the HVC Then insert the new thermocouple into the small hole see Figure 13 as far as it will go Slide the heater into the HVC until it hits the stop Make sure that the heater and thermocouple are inserted completely into the body Position the mounting block onto the side of the HVC feeding the three wires along the
6. FARRICK www harricksci com HIGH TEMPERATURE REACTION CHAMBER USER S MANUAL HARRICK SCIENTIFIC PRODUCTS INC 141 Tompkins Ave 2 floor e Pleasantville NY 10570 e 800 248 3847 e FAX 914 747 7209 d gt gt TABLE OF CONTENTS General Information LEE 1 Technical SUPPOM verted 1 gor qu 1 About the High Temperature Reaction Chamber 2 Installation and Alignment COMING READY PEE 3 Window Installation ri tite tet ertet ania eve 4 Dome Installation Pe aenea Lou abs aa eee 5 oscar 6 Fluid Electrical Connections creta el et cen ctas erre pee 7 Operation Collecting the Background Baseline Spectrum 8 Sample Spectr m 9 Options Cooling Cartridge teet E edet diee eot a Dd aee 10 miUe 12 HVC Maintenance Leak Checking 14 Cleaninigithe AVC 14 Replacing the ONGS S 14 Replacing the Heater and or Thermocouple 15 Optional and Replacement Parts 16 HVC M 7
7. hamber HVC 3 of 16 INSTALLATION AND ALIGNMENT WINDOW INSTALLATION If the windows are not already installed or need to be cleaned or changed follow the steps below Figure 2 NOTE The observation window is the window that is located between the two semicircular indentations on the rim of the dome e Insert an o ring in one of the window ports e Hold the retaining ring upside down and place a PTFE washer inside e Then carefully place a window on top of the PTFE washer e Hold the retaining ring so that it continues to retain the window and thread it into the window port e Tighten to secure the window in place using the tool provided for tightening and loosening the retaining rings e Repeat these steps until all three windows are installed NOTE careful not to touch the windows during installation Retaining Ring Window Semicircular Indentation 2 Figure 2 Installing the HVC Dome Windows 4 of 16 INSTALLATION AND ALIGNMENT DOME INSTALLATION Although it is not necessary to install the dome until later it is recommended to become familiar with the procedure before proceeding to the next step e Prior to installation of the dome make sure that the o ring and groove on the bottom of the dome are clean and free of dust e Retract the retaining plates on the HVC as far as possible e Install the dome making sure that the orientation slot on the dome engages the orientation pin on the HVC F
8. igure 3 e Slide the retaining plates all the way over the rim of the dome e Tighten the retaining plate screws to secure the dome Orientation slot Figure 3 Installing the HVC Dome 5 of 16 INSTALLATION AND ALIGNMENT INSTALLING THE HVC Before installing the HVC in the Praying Mantis make sure that the Praying Mantis is aligned in the spectrometer e Unscrew the thumbscrew on the top plate of the Praying Mantis e Carefully swing the top plate of the Praying Mantis out of the way e Grasp the sample stage Figure 4 and unscrew its mounting screw e Slide the sample stage slightly to the left to dislocate its mounting pins e Remove the sample stage e Locate the mounting pins on the side of the HVC in the pin holes where the sample stage was located e Reinstall and tighten the sample stage mounting screw Mounting Screw Sample stage Mounting Pins 2 Figure 4 Installing the HVC 6 of 16 INSTALLATION AND ALIGNMENT Gas Inlet Outlet Gas Outlet Thermocouple Cooling Heater Ports Gas Inlet Outlet Figure 5 The HVC Installed FLUID ELECTRICAL e f temperature control is desired connect the CONNECTIONS thermocouple and the heater Figure 5 to a suitable temperature controller e f the HVC is to be operated at temperatures above 100 C use 1 4 tubing to connect the two cooling ports see Figure 5 to a water inlet outlet or a coolant circu
9. lator If needed use a hose clamp to secure the tubing to the barbed fitting e f vacuum is desired connect the gas outlet 1 4 VCO fitting see Figure 5 to a vacuum pump or other source of vacuum using 3 8 1 0 vacuum tubing Seal off the two gas inlet outlet ports e If reaction or process gas es are to be passed through the sample connect the gas inlet out ports 1 4 VCO fitting see Figure 5 as needed to the gas source s Connect the gas outlet and seal off any unused gas ports e If reaction or process gas es are to be passed over the sample seal off the gas outlet Connect one of the gas inlet outlet ports to the gas source and the other as the outlet NOTE Operation above 800 C increases the thermal stress on the o rings and windows Be sure to check their condition regularly during high temperature operation Continued operation at or near the high temperature limit of the cell will reduce the lifetime of the heater A CAUTION Do not overtighten the VCO fittings These are o ring sealed fittings and they only need to be finger tight to seal If this is not sufficient inspect the o ring and replace as needed 7 of 16 7 HARRICK gt gt COLLECTING THE BACKGROUND BASELINE SPECTRUM OPERATION Place a sample screen into the sample cup and locate the plastic overflow tray over the sample cup Figure 6 Fill the sample cup with the reference material using the provided packing tool Draw
10. ls the temperature of the outer surface of the chamber and windows during high or low temperature operation The reaction chamber has three gas ports for evacuating pressurizing or flowing gas through the sample These ports are equipped with 1 4 VCO fittings One of the ports leads directly under the sample cup the other two lead into the sides of the chamber The chamber is enclosed with a dome with three windows two for the spectrometer radiation to enter and exit the chamber and the third for viewing illuminating or irradiating the sample This enables the use of the reaction chambers for photochemical studies For IR operation the standard material for the observation window is UV quartz and KBr for the other two windows For UV VIS operation the standard material for all three windows is UV quartz A CAUTION Parts for the high pressure and low pressure domes should not be exchanged The high pressure domes undergo high pressure testing and are guaranteed to work under the rated pressure 2 of 16 P d P4 HARRICK x gt INSTALLATION AND ALIGNMENT GETTING READY Before installing the High Temperature Reaction Chamber HVC familiarize yourself with it by referring to the drawing of the HVC found below Figure 1 HVC Dome Gas Inlet Outlet Gas Outlet Mounting pins 2 Thermocouple Connector Gas Inlet Outlet Heater Connector Heater Access Hole Figure 1 The High Temperature Reaction C
11. recess in the block Then use a 3 32 ball driver to secure the mounting block in place Reinstall the clamp to secure the wires to the back of the HVC Mounting Block Thermocouple Thermocouple Hole 77 sow e E Ne Heater Hole Figure 13 Installing the Heating Cartridge and or Thermocouple 15 of 16 4 4 aN g OPTIONAL PARTS Temperature Controller 110V input 24V ATC 024 3 Temperature Controller 220V input 24V ATC 024 4 RS 485 to USB Adapter for the Temperature Controller ATC USB 485 Vacuum Pump 1 VPE 001 Vacuum Pump 220V ited wiv dialed ele e AR a aa a lide ad VPE 002 High Pressure Dome for the HVC DRP ZnS Windows HVC DWI 3 High Pressure Dome for the HVC DRP ZnSe Windows HVC DWM 3 High Pressure Dome for the HVC DRP UV Quartz Windows HVC DWA 3 ZnS Window for the HVC DRP High Pressure Dome WID U43 ZnSe Window for the HVC DRP High Pressure Dome WMD U43 UV Quartz Window for the HVC DRP High Pressure Dome
12. ridge NOTE The purge shield is transparent allowing easy viewing of the sample It is not however intended for use in conjunction with sample illumination through the observation window 12 of 16 OPTIONS Feed the HVC through the purge shield Locate the mounting pins on the side of the HVC in the pin holes where the sample stage was located Reinstall and tighten the sample stage mounting screw Push the purge shield slider down to seal the front of the HVC Continue setting up the HVC as described previously Figure 11 Removing the Heating Cartridge 13 of 16 4 HARRICK gt LEAK CHECKING CLEANING THE HVC REPLACING THE O RINGS 4 HVC MAINTENANCE The HVC has been carefully checked for leaks before shipment However each time the HVC is disassembled and reassembled leaks may develop due to improper setting of the o rings If leaks occur carefully inspect all o rings and sealing surfaces for damage contamination Small leaks can be pinpointed using a Helium Leak Detector Contact Harrick Scientific Products Inc for advice and or repair information To thoroughly clean the HVC follow the procedure below e Vacuum out the sample or remove the HVC from the Praying Mantis remove the dome turn the HVC upside down and dump out the sample e Use solvent to clean off the remaining sample e Unscrew the eight screws that secure the bottom cover of the HVC e Remove the bottom cover to
13. the straightedge across the top of the cup to level off the surface Carefully remove the overflow tray Install the dome on the HVC Swing the Praying Mantis cover back into place and tighten the thumbscrew Set the temperature and pressure to desired operating conditions Set the spectrometer to measure the energy on the detector for IR operation For UV VIS spectrometers with a micro switch with the spectrometer in T mode hold the micro switch to activate the detector Adjust the micrometer to maximize the signal on the detector Collect the background spectrum Sample Cup Overflow Tray Figure 6 Filling the Cup NOTE For best results the reference material a non absorbing powder or rough surfaced solid should be ground as finely as possible and packed tightly into the sample cup 8 of 16 SAMPLE SPECTRUM OPERATION Restore the reference material to ambient conditions Remove the dome Empty the sample cup This can be done by vacuuming out the reference sample or by removing the HVC from the Praying Mantis and dumping out the material If needed clean the sample cup Fill the sample cup with the sample follow procedure in the alignment section Install the dome Install the HVC into the Praying Mantis if it was removed to empty the sample cup Swing the top plate back into place and tighten the thumbscrew Restore the desired sampling conditions Collect the sample spectr
14. um Empty the sample cup and clean it before running the next sample NOTE For best results use powdered samples in low concentration diluting as needed with a non absorbing powder such as that used for the reference 9 of 16 7 4 gt ABOUT THE COOLING CARTRIDGE INSTALLATION REMOVING THE HEATER OPTIONS This optional cooling cartridge is designed to slide into the HVC instead of the supplied heater for moderate heating or cooling of the sample It readily connects to chillers or recirculators using 74 ID tubing Clamp Clamping Screw 5 Remove the HVC from the Praying Mantis if it is installed Use a 3 32 ball driver to unfasten the screw in the mounting block on the side of the HVC and remove the mounting block Use a flat blade screwdriver to remove the screw and clamp on the back of the HVC that anchors the heater and thermocouple wire to the HVC Push a small blunt object through the heater access hole at the front of the HVC Slide the heater out the back of the unit Locate the mounting block on its pins with the thermocouple wire passing through the slot Use a 3 32 hex head driver to screw the mounting block back onto the side of the HVC Use the new thermocouple TC clamp provided to re secure the thermocouple wire Mounting Block Figure 7 Removing the Heating Cartridge 10 of 16 OPTIONS INSTALLING THE COOLING e Slide it into the HVC until it hits the stop
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