Install the Nickel Catalyst Tube
Contents
1. Installation and Operating Guide Nickel Catalyst Tube Accessory 19205A E Agilent Technologies Agilent Technologies 2000 All Rights Reserved Reproduction adaptation or translation without permission is prohibited except as allowed under the copyright laws Part number 19205 90107 First Edition DEC 2000 Replaces Part No 19205 90100 Operating and Service Manual HP is a registered trademark of Hewlett Packard Co Printed in USA Safety Information The Agilent Technologies Nickel Catalyst Tube meets the following IEC International Electrotechnical Commission classifications Safety Class 1 Transient Overvoltage Category Il and Pollution Degree 2 This unit has been designed and tested in accordance with recognized safety standards and designed for use indoors If the instrument is used in a manner not specified by the manufacturer the protection provided by the instrument may be impaired Whenever the safety protection of the Agilent 19205 has been compromised disconnect the unit from all power sources and secure the unit against unintended operation Refer servicing to qualified service personnel Substituting parts or performing any unauthorized modification to the instrument may result in a safety hazard Disconnect the AC power cord before removing covers The customer should not attempt to replace the battery or fuses in this instrument Safety Symbols Warnings in the manual or on th2. 2 to 3 4 turn Nickel catalyst Nickel catalyst exit tube inlet tube H Ny Gas sample a Tube retaining nut valve f nnnann Hg PorapakQ 4 column 6 Install the nickel catalyst inlet tube to the column bracket on the right side of the oven 7 Install the 6 ft Porapak Q column between the gas sampling valve fitting on the inlet side of the oven and the nickel catalyst inlet tube on the detector side of the oven WARNING Hydrogen H5 is flammable and is an explosion hazard when confined in an enclosed space for example the oven In any application using H turn off the supply at its source before working on the instrument 8 Turn offthe hydrogen at its source Locate the hydrogen line marked in red at the flow manifold that feeds the FID being used Trace the line to the area behind the nickel catalyst tube Using a suitable tubing The Nickel Catalyst Tube Accessory 19205A Install the Nickel Catalyst Tube cutting tool carefully cut the hydrogen line Be careful not to crush the tubing while cutting it Hydrogen supply to FID Hydrogen supply to Nickel Catalyst m di Plugged 1 16 inch union 1 16 inch union C ZA 7 AU d E A I a 74 nes jp Hydrogen line Marked in red 9 Using the stainless steel 1 16 inch union provided connect the hydrogen supply side of the line to one side of the union Insert t
3. A position 2 Using the next figure as a guide install the Nickel Catalyst tube from the top of the oven Use the insulation removed tear apart as needed to fill in the area around the Nickel Catalyst Tube The Nickel Catalyst Tube Accessory 19205A Install the Nickel Catalyst Tube 3 Install the cover plate provided Secure the cover plate with two M4 Screws M4 screws GET N AS Cover plate H3 inlet tube To right column mounting bracket The Nickel Catalyst Tube Accessory 19205A Install the Nickel Catalyst Tube 4 Place the three pieces of insulation in the insulation cup Install the cup over the carrier gas tubing and nickel catalyst tube inside the oven Secure the cup using two M4 screws provided 4 MI s 4 Nm i 1 I 1 I I l 1 I l I I 1 D onnAnn An n amp Io FID To right column mounting bracket hoa Oo OUI 5 Connect the nickel catalyst exit tube to the FID inlet Assemble a 1 8 inch stainless steel nut and front and back ferrule onto the tubing Fully insert the tube ferrules and nut onto the FID base Tighten the The Nickel Catalyst Tube Accessory 19205A Install the Nickel Catalyst Tube nut finger tight Use a wrench to tighten the nut an additional 1
4. hazard when confined in an enclosed space for example the oven 13 Restore carrier gas flow and leak test the new installation 14 Reinstall the panels and covers Reconnect the instrument power cord and restore power The Nickel Catalyst Tube Accessory 19205A Operation Operation Verifying Performance l Ifany heated zone is turned on turn it off and allow it to cool DO NOT heat any heated zone 2 Setthe gas flows Table 1 For a standard FID installation Flow mL min Carrier flow helium 30 FID hydrogen flow 30 FID air flow 400 Table 2 If there is a TCD FID in series installation Flow mL min Carrier flow helium 30 TCD switching flow 25 FID hydrogen flow 45 FID air flow 500 Allow helium and hydrogen to flow through the system for 15 minutes 4 Carefully check the column and supply fittings for leaks Air leaks can damage the catalyst 5 Condition the nickel catalyst by setting the nickel catalyst tube temperature INJ B TEMP to 375 C and the FID temperature to 400 C Allow them to condition for 1 hour While the zones are heating ignite the FID flame The Nickel Catalyst Tube Accessory 19205A Operation 6 After 1 hour set the following temperature Setting C Oven temperature 35 FID temperature as desired Nickel catalyst 375 TCD if in use as desired When the temperatures have st
5. abilized the system is ready for use 7 Load the sample loop with the nickel catalyst test mixture a quick press of the can button and start the run The chromatogram should be similar to the one in the figure below CO may be larger due to the presence of air in the sample START IF STOP Using the Nickel Catalyst 1484 CO CHa To use the Nickel Catalyst accessory most efficiently keep the following in mind e Avoid exposing the catalyst to oxygen which can damage it e If performance is significantly degraded repack the catalyst tube WARNING WARNING WARNING Caution The Nickel Catalyst Tube Accessory 19205A Maintenance Maintenance Repacking the Catalyst Should it be necessary to repack the nickel catalyst tube because of loss of conversion efficiency repack the catalyst as described below Hydrogen H5 is flammable and is an explosion hazard when confined in an enclosed space for example the oven In any application using H turn off the supply at its source before working on the instrument Both nickel oxide and some forms of silicon oxide are considered carcinogens for humans It is important to perform all work in a fume hood and to wear cotton gloves at all times Remove any spills with a HEPA type vacuum cleaner avoiding any action that creates dust Alert your company s safety group when a spill is created Due to the possibility of dermatitis wash the arms and hands w
6. alyst assembly upside down and add catalyst slowly Tap gently on the tube to help seat it properly When the catalyst is 22 mm from the end stop adding catalyst Do NOT crush the catalyst when packing or measuring the depth 14 Add a single glass wool plug to fill the remaining part of the tube to within 5 mm of the end This plug should be gently compressed during installation Before installing the catalyst assembly into the oven carefully wipe it to remove any catalyst dust 15 Reassembly of the nickel catalyst is the reverse of steps 1 through 6 The Nickel Catalyst Tube Accessory 19205A Maintenance WARNING Make sure that the insulation is carefully repacked around the tube before you reinstall the injector cover plate and the capillary retainer cup 16 Leak test the new installation WARNING Hydrogen H5 is flammable and is an explosion hazard when confined in an enclosed space for example the oven 17 Start the carrier and hydrogen flows then allow them to flow for 15 minutes 18 Heat the nickel catalyst to 375 C and hold for 30 minutes The accessory should be ready for use Replacement Parts List Ref Name Part No Number 1 Packed Catalyst Tube Assembly 18900 61020 2 Reducer 0100 0073 3 H Mix Weldment 18900 80820 4 520mm 1 16 inch Tube with 1 8 inch end 1530 2167 5 Nut Front ferrule and Back ferrule SS 1 4 inch kit of 20 5080 8753 6 1 16 inch x 1 16 inch SS Unio
7. e instrument must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions violates safety standards of design and the intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements WARNING A warning calls attention to a condition or possible situation that could cause injury to the user CAUTION A caution calls attention to a condition or possible situation that could damage or destroy the product or the user s work Sound Emission Certification for Federal Republic of Germany Sound pressure Lp 68 dB A During normal operation At the operator position According to ISO 7779 Type Test Schallemission Schalldruckpegel LP 68 dB A Am Arbeitsplatz Normaler Betrieb Nach DIN 45635 T 19 Typpr fung Agilent Technologies Inc 2850 Centerville Road Wilmington DE 19808 1610 USA The Nickel Catalyst Tube Accessory 19205A WARNING The 19205A Nickel Catalyst Tube Accessory is used on the 4890 5890 gas chromatographs for trace analysis of CO and CO using a Flame Ionization Detector FID The gas sample is separated on the column then passes over the hot catalyst in the presence of hydrogen so that the CO and CO are converted to CH4 The Nickel Catalyst Tube Accessory is installed in the inlet B position These instructions describe installation of the accessory for
8. he tube into the fitting fully Use a wrench to tighten the nut 1 2 to 3 4 turn past finger tight 10 Insert the 1 16 inch hydrogen supply tube from the nickel catalyst tube into the other end of the union and tighten as described above 11 Install the plugged union provided on the hydrogen line from the FID detector The Nickel Catalyst Tube Accessory 19205A Install the Nickel Catalyst Tube 12 Route the heater and sensor wires through the cable tray behind the oven to the main circuit board Install the pins in the B injection port connector positions 4890 Series and 5890 SERIES II Main Circuit Board Connect the sensor leads white to P7 heater leads red to J9 Sendors EI mmm aue Heaters i jemois 2 jrorses 4 mass L J9 L joris B EA oe iD 6 Position 3 amp 4 Inj B position The Nickel Catalyst Tube Accessory 19205A Install the Nickel Catalyst Tube 5890A Main Circuit Board Connect the sensor leads white to J7 heater leads red to J9 asoa Da 0501 y White STRT 11 amp 125 Door 13 amp 14 m Z a manwa c ao ote Position 9 amp 10 Inj B position Cryo 142 INI B 3642 LINT A 5 amp J9 Det B 7885 Heaters Det A 9 amp 0 sition 3 amp 4 Inj B position Red P o WARNING Hydrogen H5 is flammable and is an explosion
9. ith soap and water after use The use of long sleeves is required during any use and spill cleanup If long sleeves are not worn long gloves are an acceptable substitute After the assembly is filled with catalyst the whole assembly should be carefully wiped to remove any catalyst dust Be sure to read the Material Safety Data Sheet MSDS provided with the catalyst before performing this procedure 1 Turnoffthe INJ B TEMP Turn offall other heaters When the nickel catalyst tube is cooled to room temperature turn off the power to the GC and disconnect the power cord Bleed down the hydrogen and carrier gas 2 Use a Pozidrive screwdriver to remove the two screws holding the injector cover plate on top of the nickel catalyst tube Remove the plate and the insulation around the nickel catalyst tube The Nickel Catalyst Tube Accessory 19205A Maintenance From inside the oven loosen the two screws holding the capillary retainer cup rotate the cup and allow it to drop away from the base of the nickel catalyst assembly Refer to the following figure which shows the nickel catalyst assembly and the packed catalyst assembly Use two wrenches to disconnect the H mix weldment 5 from the bottom of the packed catalyst assembly 1 Be very careful NOT to place stress on the 1 16 inch tube Stress can damage the weldment Packed catalyst tube Packed area Use two wrenches to disconnect the reducer 2 from the top
10. n 0100 0124 7 Brass Cap seal 1 8 inch Supplied with replacement 8 Polyethylene Cap Supplied with replacement 9 Nut Front ferrule and Back ferrule SS 1 8 inch kit of 20 5080 8751 10 Nut Front ferrule and Back ferrule SS 1 16 inch kit of 10 5180 4149 The Nickel Catalyst Tube Accessory 19205A Maintenance ns NICAT Test Sample pressurized can 19354 60510 ns Injector Cover Plate 19243 00050 ns Capillary Retainer Cup 19243 00070 ns Insulation for Cup 3 required 19243 00067 ns Column Bulkhead Fitting and Tube 07675 80050 ns Retaining Nut for Bulkhead Fitting 2950 0203 ns 6 ft x 1 8 inch OD Porapak Q Column 19006 80015 The Nickel Catalyst Tube Accessory 19205A Maintenance 20 RES Agilent Technologies Printed on recycled paper This product is recyclable Agilent Technologies Inc Printed in USA Dec 2000 19205 90107
11. of the packed catalyst assembly 1 Gently lift the packed catalyst assembly 1 out of the injection area Both ends of the catalyst tube are now accessible WARNING Caution The Nickel Catalyst Tube Accessory 19205A Maintenance 7 With a hooked instrument of some type carefully remove the glass wool plug from the bottom of the tube Make sure you get all of it 8 Empty the old catalyst from the tube you may have to break it out with a pointed tool Make sure you get it all out 9 Using a thin rod push out the top glass wool plug from the tube 10 Clean the inside of the tube thoroughly with methanol Do not use any sharp metal tools on the inside of the tube A cotton swab carefully used will assure cleanliness Dry the tube The figure above shows the dimensions for repacking the tube correctly If any catalyst is outside the heated zone severe tailing of CO will result ll Prepare a simple depth gage using a wooden cotton swab or any other handy rod or tubing Use tape or paint to mark the stick at 46 mm and at 22 mm from the blunt end 12 Roll up a piece of glass wool into a ball about the size of a large pea Push this into the tube from the 1 4 inch end and seat it firmly Measure the depth of this glass wool with the depth guage it should be 46 mm from the end of the tube If necessary add more glass wool A slight compression of the glass wool during the measurement works best 13 Turn the nickel cat
12. two tray locks that hold it in position then sliding the tray away from the instrument b Liftthe autosampler tray from its mounting bracket and set it aside The Nickel Catalyst Tube Accessory 19205A Prepare the Instrument c Remove the autosampler bracket by removing the six screws securing it to the instrument Left side panel 8 Remove the two screws securing the left side panel along its bottom edge 9 Slide the left side panel towards the rear of the instrument and lift 10 Remove the electronics carrier top cover by grasping it at the rear and lifting upwards until its catch releases then pull it towards the rear of the instrument Electronics carrier top cover The Nickel Catalyst Tube Accessory 19205A Install the Nickel Catalyst Tube 11 Remove the right side panel by removing four screws two each along its top and bottom edges Screws Right side panel Install the Nickel Catalyst Tube The insulation on the GC is made of refractory ceramic fibers Ventilate your work area Wear long sleeves gloves safety glasses and a disposable dust mist respirator Dispose of insulation in a sealed plastic bag Caution The Nickel Catalyst Tube Accessory 19205A Install the Nickel Catalyst Tube l If present remove the cover plate from the B inlet mounting location and the pre cut insulation below it Inlet cover plate ZA Ze KEP pO eS hn m B position Pun
13. use with a gas sampling valve although the accessory can be used with any inlet Prepare the Instrument Hazardous voltages are present in the instrument whenever the power cord is connected Avoid a potentially dangerous shock hazard by disconnecting the power cord before working on the instrument Copyright 2000 Agilent Technologies Printed in USA Dec 2000 Agilent Part No G2651 90107 The Nickel Catalyst Tube Accessory 19205A Prepare the Instrument 1 Set the main power line switch to the off position Red 0 visible UL n N 0 Disconnect the power cable from its receptacle Allow time for the oven and heated zones to cool When the heated zones are cool turn off all gas supplies at the source oP WO hf Remove the column and any hardware attached to the FID liner column liner nuts ferrules makeup gas adapter etc The Nickel Catalyst Tube Accessory 19205A Prepare the Instrument 6 Remove the injection port cover by grasping its back edge and lifting it upward If an autosampler is installed the injection port cover will not be present Injection port cover Press here to free cover 1 4 inch screw and washer 7 If an autosampler is installed on the instrument it will be necessary to remove it and its mounting bracket to allow removal of the left side cover a Remove the autosampler tray from its mounting bracket by simultaneously lifting and turning the
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