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Declaration Manufacturer: Thermo Fisher Scientific Thermo Fisher Scientific is the manufacturer of the instrument described in this manual and, as such, is responsible for the instrument safety, reliability and performance only if: • installation • re-calibration • changes and repairs have been carried out by authorized personnel and if: •...
Contents About This Manual..........................xi Overview ...........................xi Conventions Used in This Manual..................xiii Instrument Markings and Symbols ..................xvi Using Hydrogen ........................xvii Using the Hydrogen Sensor ..................xviii Chapter 1 Preventive Maintenance........................21 Suggested Maintenance Schedule .................... 22 Chapter 2 Maintaining a Split/Splitless Injector ....................25 Split/Splitless Injector ......................
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Contents Cold On-Column Injector Maintenance ................100 Possible leaks in the rotary valve ................100 Chapter 6 Maintaining a Cold On-Column Injector...................111 Manual Cold On-Column Injector..................112 Cold On-Column Injector Maintenance ................114 Possible leaks in the rotary valve ................114 Chapter 7 Maintaining a Packed Column Injector ....................121 Packed Column Injector ......................
About This Manual Overview This manual reports information and operating sequences for the maintenance and the troubleshooting of the TRACE GC Ultra and its components. This manual is organized as follows: Chapter 1, Preventive Maintenance, gives a schedule for preventive maintenance of your TRACE GC Ultra.
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About This Manual Overview Chapter 11, Maintaining a FID, reports information and maintenance sequences for the Flame Ionization (FID) detector. Chapter 12, Maintaining an Electron Capture Detector, reports information and maintenance sequences for the Electron Capture (ECD) detector. Chapter 13, Maintaining a Nitrogen Phosphorus Detector, reports information and maintenance sequences for the Nitrogen Phosphorus (NPD) detector.
Conventions Used in This Manual About This Manual Conventions Used in This Manual The following symbols and typographical conventions are used throughout this manual. Bold Bold text indicates names of windows, menus, dialog boxes, buttons, and fields. Italic Italic indicates cross references, first references to important terms defined in the glossary, and special emphasis.
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About This Manual Conventions Used in This Manual This symbol indicates danger from hazardous chemicals. This symbol indicates danger from high temperature surfaces or substances. This symbol indicates a fire hazard. This symbol indicates an explosion hazard. This symbol indicates a toxic hazard. This symbol indicates the presence of flammable materials.
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Conventions Used in This Manual About This Manual This symbol indicates the user must wear protective shoes when performing the procedure. This symbol indicates the user must wear protective clothing when performing the procedure. This symbol indicates the user must wear gloves when performing the procedure.
About This Manual Instrument Markings and Symbols Instrument Markings and Symbols The following table explains the symbols used on Thermo Fisher Scientific instruments. Only a few of them are used on the TRACE GC Ultra. Symbol Description Direct Current Alternating Current...
Using Hydrogen About This Manual Symbol Description Equipment protected throughout by DOUBLE INSULATION or REINFORCED INSULATION (Equivalent to Class II of IEC 536) Caution, risk of electric shock Caution, hot surface Caution (refer to accompanying documents) In-position of a bistable push control Out-position of a bistable push control Symbol in compliance to the Directive 2002/96/EC on Waste Electrical and Electronic Equipments (WEEE)
About This Manual Using Hydrogen Use the following safety precautions when using hydrogen: • Ensure that all hydrogen cylinders comply with the safety requirements for proper use and storage. Hydrogen cylinders and delivery systems must comply with local regulations. • Make sure the gas supply is turned completely off when connecting hydrogen lines.
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Using Hydrogen About This Manual If the sensor detects anomalies or leaks during GC operation due to instrument malfunction, the operator must immediately: • close the hydrogen supply • switch off the gas chromatograph • air out the room The reliability of the sensor depends on careful maintenance. After the sensor is in use, you must periodically check its operating performance and calibration as recommended by the manufacturer.
Chapter 1 Preventive Maintenance Suggested Maintenance Schedule Suggested Maintenance Schedule Preventive maintenance keeps your instruments running at peak performance. The recommended maintenance schedule shown in Table 1-1 on page 23 is based on a GC running multiple samples in an 8-hour day. You may need to adapt the schedule to your situation depending on: •...
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Chapter 1 Suggested Maintenance Schedule Preventive Maintenance Table 1-1. Standard Maintenance Schedule Frequency Task Daily Run performance check standard as required by method. Run calibration curve as required by method. Note gas pressure when the weekly pressure check shows it to be below 5000 kPa (50 bar or 750 psig).
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Chapter 1 Preventive Maintenance Suggested Maintenance Schedule Table 1-1. Standard Maintenance Schedule Annually Clean FID collector. Replace PID lamp. Regenerate the active carbon filter mounted on the carrier gas line Regenerate the active carbon filter mounted on the split line. Biannually Replace FPD photomultiplier.
Maintaining a Split/Splitless Injector Chapter at a Glance… Split/Splitless Injector ..................26 Split/Splitless Injector Maintenance..............28 Operating Sequences Replace the Septum ....................30 Clean or Replace the Liner ...................34 Replace a Broken Liner ..................40 Replace the Split Line Tubing ................48 Maintenance and Troubleshooting Manual...
Chapter 2 Split/Splitless Injector Maintenance Maintaining a Split/Splitless Injector You can replace the liner with a new one or clean the liner and reinstall it. Table 2-2, S/SL available liners, shows the available types of liners and the indications for the correct choice. This operating sequence describes how to: •...
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Chapter 2 Maintaining a Split/Splitless Injector Replace the Septum OPERATING SEQUENCE Replace the Septum Materials needed • Non metallic sharp tool • Septum (P/N 313 032 11) • Tweezers WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the injector must be cooled to room temperature.
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Chapter 2 Replace the Septum Maintaining a Split/Splitless Injector 5. When the inlet reaches the room temperature, RIGHT CARRIER (S/SL) press LEFT CARRIER RIGHT CARRIER depending on which injector is operating. Pressure 30.0 30.0 Col. flow 3.00 < 6. Scroll to and press Pressure Lin.
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Chapter 2 Maintaining a Split/Splitless Injector Replace the Septum 9. Remove the septum from the septum holder (use non-metallic tools) 10. Insert a new septum into the septum holder. CAUTION Use tweezers to avoid touching the septum with your fingers. 11.
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Chapter 2 Replace the Septum Maintaining a Split/Splitless Injector 16. Press LEFT INLET or RIGHT INLET, depending on which injector is operating, scroll to Temp press ON. 17. Perform a leak check according to Performing a Leak Check (Capillary Column) Operating Sequence on page 181.
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Chapter 2 Maintaining a Split/Splitless Injector Clean or Replace the Liner OPERATING SEQUENCE Clean or Replace the Liner Materials needed • Liner cap removal tool (P/N 205 070 10) • Glass liner (see Table 2-2, on page 29) • Graphite seal (P/N 290 334 06) •...
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Chapter 2 Clean or Replace the Liner Maintaining a Split/Splitless Injector 3. Press LEFT INLET or RIGHT INLET depending on RIGHT INLET (S/SL) which injector is operating. In the following example, a S/SL injector installed on the right Temp 250 < channel is considered.
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Chapter 2 Maintaining a Split/Splitless Injector Clean or Replace the Liner 9. Use the liner cap wrench provided with the GC to remove the injector liner cap. 10. Use tweezers to remove the liner with the graphite seal. CAUTION Be careful not to break the glass liner inside the injector when removing it.
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Chapter 2 Clean or Replace the Liner Maintaining a Split/Splitless Injector 12. Using tweezers, remove the liner from the bath and dry it with compressed clean air. NOTE For trace analysis, you should pre- treat the liner with a suitable silylating reagent prior to re- inserting it into the injector.
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Chapter 2 Maintaining a Split/Splitless Injector Clean or Replace the Liner 15. Tighten the liner cap using the liner cap wrench provided with the GC. 16. Remove the septum from the septum holder (use non-metallic tools). 17. Insert a new septum into the septum holder. CAUTION Use tweezers to avoid touching the septum with your fingers.
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Chapter 2 Clean or Replace the Liner Maintaining a Split/Splitless Injector 18. Clean the septum support from possible fragments left by the septum and reinsert it into the injector 19. Place the septum holder on the top of the septum support. 20.
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Chapter 2 Maintaining a Split/Splitless Injector Replace a Broken Liner OPERATING SEQUENCE Replace a Broken Liner Materials needed • Liner cap removal tool (P/N 205 070 10) • Glass liner (see Table 2-2 on page 29) • Tweezers WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the injector must be cooled to room temperature.
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Chapter 2 Replace a Broken Liner Maintaining a Split/Splitless Injector 5. When the inlet reaches the room temperature, RIGHT CARRIER (S/SL) press LEFT CARRIER RIGHT CARRIER depending on which injector is operating. Pressure 30.0 30.0 Col. flow 3.00 < 6. Scroll to and press Pressure Lin.
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Chapter 2 Maintaining a Split/Splitless Injector Replace a Broken Liner 9. Use the liner cap wrench provided with the GC to remove the injector liner cap. 10. Use tweezers to remove the upper part of the broken liner (with the graphite seal) from the injector.
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Chapter 2 Replace a Broken Liner Maintaining a Split/Splitless Injector 11. Unscrew the nut that retains the analytical column. 12. Remove the analytical column with its ferrule. 13. Unscrew the retaining nut at the bottom of the injector. 14. Remove the terminal fitting with its silver seal. CAUTION Glass splinters from the broken liner will fall from the injector.
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Chapter 2 Maintaining a Split/Splitless Injector Replace a Broken Liner 16. Reinsert the silver seal and the terminal fitting. 17. Tighten the nut that retains the terminal fitting. 18. Insert the analytical column with its ferrule into the bottom of the injector in its previous ™...
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Chapter 2 Replace a Broken Liner Maintaining a Split/Splitless Injector 20. Holding the new liner with tweezers, place a graphite seal over the liner, making sure to leave a distance of about 10 mm between the seal and the liner end. 21.
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Chapter 2 Maintaining a Split/Splitless Injector Replace a Broken Liner 23. Remove the septum from the septum holder (use non-metallic tools). 24. Insert a new septum into the septum holder. CAUTION Use tweezers to avoid touching the septum with your fingers. 25.
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Chapter 2 Replace a Broken Liner Maintaining a Split/Splitless Injector 30. Press LEFT INLET or RIGHT INLET, depending on which injector is operating, scroll to Temp press ON. 31. Perform a leak check according to Performing a Leak Check (Capillary Column) Operating Sequence on page 181.
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OPERATING SEQUENCE Replace the Split Line Tubing Materials needed • 7/16” wrenches • Two 8-10 mm wrences • Kit Assy Split line 1/8” (PN 190 507 00) — Split line tubing 1/8” — Brass front/back ferrule for 1/8” tubing — 5/16”...
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Chapter 2 Replace the Split Line Tubing Maintaining a Split/Splitless Injector and press OFF. 4. Scroll to Temp 5. When the inlet reaches the room temperature, RIGHT CARRIER (S/SL) press LEFT CARRIER RIGHT CARRIER depending on which injector is operating. Pressure 30.0 30.0...
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Chapter 2 Maintaining a Split/Splitless Injector Replace the Split Line Tubing Disconnect the split line tubing from the injector body and from the split line filter. a. Using the 7/16” wrench, unscrew and disconnect the split line tubing from the injection body.
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Chapter 2 Replace the Split Line Tubing Maintaining a Split/Splitless Injector 11. Connect the new split line tubing to the injector body. a. On the end of the new split line tubing having the greater diameter, slide the 5/16” brass nut and the brass front/back ferrule. b.
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Chapter 2 Maintaining a Split/Splitless Injector Replace the Split Line Tubing 15. Press LEFT INLET or RIGHT INLET, depending on which injector is operating, scroll to Temp press ON. 16. Perform a leak check according to Performing a Leak Check (Capillary Column) Operating Sequence on page 181.If leaks are detected, check the critical connections with an electronic...
Maintaining a Large Volume Splitless Injector Chapter at a Glance… Large Volume Splitless Injector ................54 Large Volume Splitless Injector Maintenance............56 Operating Sequences Replace the Septum ....................58 Clean or Replace the Liner ...................61 Replace a Broken Liner ..................67 Replace the Split Line Tubing ................74 Maintenance and Troubleshooting Manual...
Chapter 3 Maintaining a Large Volume Splitless Injector Large Volume Splitless Injector Large Volume Splitless Injector Maintenance and Troubleshooting Manual...
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Chapter 3 Large Volume Splitless Injector Maintaining a Large Volume Splitless Injector Table 3-1. Large Volume Splitless Injector spare parts Description Qty. Septum Cap 3500 13 25 11-mm OD BTO Septum with center guide 313 032 35 Ring Nut 350 013 24 Septum Holder 247 520 26 O-ring...
Chapter 3 Maintaining a Large Volume Splitless Injector Large Volume Splitless Injector Maintenance Large Volume Splitless Injector Maintenance The LVSL (Large Volume Splitless) injector will normally be serviced by Thermo Fisher Scientific authorized technical personnel. In order to operate at peak performances, the injector requires periodic maintenance from the user.
Chapter 3 Large Volume Splitless Injector Maintenance Maintaining a Large Volume Splitless Injector Table 3-2. LVSL available liners Application Glass liner packed with deactivated glass wool 453 220 65 Deactivated laminar liner (optional) 453 220 67 If the glass liner breaks inside the injector When replacing or removing a glass liner, it might break inside the injector.
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Chapter 3 Maintaining a Large Volume Splitless Injector Replace the Septum OPERATING SEQUENCE Replace the Septum Materials needed • Non metallic sharp tool • Septum (P/N 313 032 41) • Tweezers WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the injector must be cooled to room temperature.
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Chapter 3 Replace the Septum Maintaining a Large Volume Splitless Injector 5. When the inlet reaches the room temperature, RIGHT CARRIER (S/SL) press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating. Pressure 30.0 30.0 Col. flow 3.00 <...
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Chapter 3 Maintaining a Large Volume Splitless Injector Replace the Septum 9. Insert a new septum into the septum holder. CAUTION Use tweezers to avoid touching the septum with your fingers. 10. Tighten the injector cap to finger tight. CAUTION Do not overtighten the injector cap.
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Chapter 3 Clean or Replace the Liner Maintaining a Large Volume Splitless Injector OPERATING SEQUENCE Clean or Replace the Liner Materials needed • Liner cap removal tool (P/N 205 070 10) • Glass liner (see Table 3-2, on page 57) •...
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Chapter 3 Maintaining a Large Volume Splitless Injector Clean or Replace the Liner 3. Press LEFT INLET or RIGHT INLET depending on RIGHT INLET (S/SL) which injector is operating. In the following example, a S/SL injector installed on the right Temp 250 <...
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Chapter 3 Clean or Replace the Liner Maintaining a Large Volume Splitless Injector 9. Use the liner cap wrench provided with the GC to remove the injector liner cap. 10. Use tweezers to remove the liner with the graphite seal. CAUTION Be careful not to break the glass liner inside the injector when...
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Chapter 3 Maintaining a Large Volume Splitless Injector Clean or Replace the Liner 12. Using tweezers, remove the liner from the bath and dry it with compressed clean air. NOTE For trace analysis, you should pre- treat the liner with a suitable silylating reagent prior to re- inserting it into the injector.
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Chapter 3 Clean or Replace the Liner Maintaining a Large Volume Splitless Injector 14. Tighten the liner cap using the liner cap wrench provided with the GC. 15. Place the septum holder with the septum onto the inlet port, then screw and tighten the ring nut up to the stop.
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Chapter 3 Maintaining a Large Volume Splitless Injector Clean or Replace the Liner 17. Press LEFT CARRIER or RIGHT CARRIER, depending on which injector is operating, scroll and press ON. Pressure 18. Press OVEN, scroll to and press ON. Temp 19.
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Chapter 3 Replace a Broken Liner Maintaining a Large Volume Splitless Injector OPERATING SEQUENCE Replace a Broken Liner Materials needed • Liner cap removal tool (P/N 205 070 10) • Glass liner (see Table 3-2 on page 57) • Tweezers WARNING! This operation must be carried out at low temperature to avoid burns.
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Chapter 3 Maintaining a Large Volume Splitless Injector Replace a Broken Liner 5. When the inlet reaches the room temperature, RIGHT CARRIER (S/SL) press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating. Pressure 30.0 30.0 Col. flow 3.00 <...
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Chapter 3 Replace a Broken Liner Maintaining a Large Volume Splitless Injector 10. Use tweezers to remove the upper part of the broken liner (with the graphite seal) from the injector. 11. Unscrew the nut that retains the analytical column. 12.
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Chapter 3 Maintaining a Large Volume Splitless Injector Replace a Broken Liner 13. Unscrew the retaining nut at the bottom of the injector. 14. Remove the terminal fitting with its silver seal. CAUTION Glass splinters from the broken liner will fall from the injector. 15.
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Chapter 3 Replace a Broken Liner Maintaining a Large Volume Splitless Injector 18. Insert the analytical column with its ferrule into the bottom of the injector in its previous ™ position (for instructions, refer to the TRACE GC Operating Manual). 19.
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Chapter 3 Maintaining a Large Volume Splitless Injector Replace a Broken Liner 21. Tighten the liner cap using the liner cap wrench provided with the GC. 22. Place the septum holder with the septum onto the inlet port, then screw and tighten the ring nut up to the stop.
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Chapter 3 Replace a Broken Liner Maintaining a Large Volume Splitless Injector 25. Press OVEN, scroll to and press ON. Temp 26. Press LEFT INLET or RIGHT INLET, depending on which injector is operating, scroll to Temp press ON. 27. Perform a leak check according to Performing a Leak Check (Capillary Column) Operating...
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Chapter 3 Maintaining a Large Volume Splitless Injector Replace the Split Line Tubing OPERATING SEQUENCE Replace the Split Line Tubing Materials needed • 7/16” wrenches • Two 8-10 mm wrences • Kit Assy Split line 1/16” (PN 190 507 10) —...
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Chapter 3 Replace the Split Line Tubing Maintaining a Large Volume Splitless Injector and press OFF. 4. Scroll to Temp 5. When the inlet reaches the room temperature, RIGHT CARRIER (S/SL) press LEFT CARRIER RIGHT CARRIER depending on which injector is operating. Pressure 30.0 30.0...
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Chapter 3 Maintaining a Large Volume Splitless Injector Replace the Split Line Tubing Disconnect the split line tubing from the injector body and from the split line filter. a. Using the 7/16” wrench, unscrew and disconnect the split line tubing from the injection body.
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Chapter 3 Replace the Split Line Tubing Maintaining a Large Volume Splitless Injector 11. Connect the new split line tubing to the injector body. a. On the end of the new split line tubing having the greater diameter, slide the 5/16” brass nut and the brass front/back ferrule.
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Chapter 3 Maintaining a Large Volume Splitless Injector Replace the Split Line Tubing 12. Connect the new split line tubing to the split line dummy filter a. On the end of the new split line tubing having the lower diameter, slide the nut 6MB nut and the 1.6 mm ID brass ferrule.
Maintaining a Cold On-Column Injector for Standard Automatic Injections This inlet works in combination with the TriPlus autosampler allowing standard injections into a 0.53-mm ID capillary column. Chapter at a Glance… Automated Operation Cold On-Column Injector ..........80 Cold On-Column Injector Maintenance ...............82 Operating Sequences Replace the O-Ring...
Chapter 4 Maintaining a Cold On-Column Injector for Standard Automatic Injections Cold On-Column Injector Maintenance Cold On-Column Injector Maintenance This injector will normally be serviced by Thermo Fisher Scientific authorized technical personnel and do not require periodic maintenance, except for O-ring replacement in the automatic version.
Chapter 4 Replace the O-Ring Maintaining a Cold On-Column Injector for Standard Automatic Injections OPERATING SEQUENCE Replace the O-Ring NOTE This sequence is used for the Automated Operation Cold On-Column Injector for TriPlus Sampler. Materials needed • Flat screwdriver • O-Ring (See # 5, Table 4-1 on page 81) •...
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Chapter 4 Maintaining a Cold On-Column Injector for Standard Automatic Injections Replace the O-Ring 5. Unscrew the seal holder and remove it. 6. Remove the O-ring from the seal holder with the aid of a sharp, non-metallic tool. 7. Insert a new O-ring in the relevant seat. CAUTION Use tweezers to avoid touching the O-ring with your fingers.
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Chapter 4 Replace the O-Ring Maintaining a Cold On-Column Injector for Standard Automatic Injections 8. Screw and tighten the seal holder onto its housing. CAUTION Tightening of the seal holder must be performed carefully in order to properly seal the On- Column needle guide.
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Chapter 4 Maintaining a Cold On-Column Injector for Standard Automatic Injections Replace the O-Ring 10. Press LEFT CARRIER or RIGHT CARRIER, depending on which injector is operating, scroll and press ON. Pressure 11. Press OVEN, scroll to and press ON. Temp 12.
Chapter 4 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector for Standard Automatic Injections OPERATING SEQUENCE Replace the Rotary Valve Seal Materials needed • 5.5 mm hexagonal wrench • PTFE seal (P/N 290 070 01) • 3 mm Allen wrench •...
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Chapter 4 Maintaining a Cold On-Column Injector for Standard Automatic Injections Replace the Rotary Valve Seal 6. Disconnect the cables coming from the actuator and the TriPlus sampler from the control interface. 7. Remove the actuator body and the ground wire fixing screw....
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Chapter 4 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector for Standard Automatic Injections 8. Move vertically the valve lever to allows its extraction through the slot on the actuator shaft. Carefully lift up the automatic actuator to remove it from the OC housing.
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Chapter 4 Maintaining a Cold On-Column Injector for Standard Automatic Injections Replace the Rotary Valve Seal 10. Unscrew the two Allen bolts that fix the injector body to the injector base. Remove the injector body from its base. CAUTION Pay attention not to lose the small needle guide when removing the injector body.
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Chapter 4 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector for Standard Automatic Injections 12. Remove the clip that retains the rotary valve. 13. Push the rotary valve out from the injector head. 14. Push the PTFE seal upwards to eject it. CAUTION In order to avoid leaks of sample from the valve...
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Chapter 4 Maintaining a Cold On-Column Injector for Standard Automatic Injections Replace the Rotary Valve Seal 18. Reassemble the two parts of the injector body. 19. Remount the injector body on its base, tightening the two Allen screws. CAUTION Be careful to reinstall the needle guide with the small cut downwards, otherwise no flow of carrier gas to the column will...
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Chapter 4 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector for Standard Automatic Injections 20. . Fix the OC head on the ceiling of the GC and tighten the two screws A on the side of the OC head previously loosened.
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Chapter 4 Maintaining a Cold On-Column Injector for Standard Automatic Injections Replace the Rotary Valve Seal 22. .Adjust the position of the automatic actuator up to align the fixing holes provided on the actuator body with the corresponding fixing holes located on the fixing arm of the OC head. Fix the parts by using the two fixing screws.
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Chapter 4 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector for Standard Automatic Injections 28. Press OVEN, scroll to and press ON. Temp 29. Perform a leak check according to Performing a Leak Check (Capillary Column) Operating Sequence on page 181. From the data system in use, enable the automatic actuator to open and close the rotary valve of the OC injector by using the direct...
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Chapter 4 Maintaining a Cold On-Column Injector for Standard Automatic Injections Replace the Rotary Valve Seal Maintenance and Troubleshooting Manual...
Maintaining a Cold On-Column Injector Direct Narrow-Bore This inlet works in combination with the TriPlus autosampler allowing standard injections into a 0.25/0.32-mm. ID capillary column. Chapter at a Glance… Automated Operation Cold On-Column Injector ..........98 Cold On-Column Injector Maintenance .............100 Operating Sequences Replace the Rotary Valve Seal ................101...
Chapter 5 Maintaining a Cold On-Column Injector Direct Narrow-Bore Cold On-Column Injector Maintenance Cold On-Column Injector Maintenance This injector will normally be serviced by Thermo Fisher Scientific authorized technical personnel and do not require periodic maintenance. The PTFE seal of the rotary valve, if worn, can be replaced by the user.
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Chapter 5 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector Direct Narrow-Bore OPERATING SEQUENCE Replace the Rotary Valve Seal Materials needed • 5.5 mm hexagonal wrench • PTFE seal (P/N 29007106) • 3 mm Allen wrench • 4-mm Allen wrench •...
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Chapter 5 Maintaining a Cold On-Column Injector Direct Narrow-Bore Replace the Rotary Valve Seal 6. Disconnect the cables coming from the actuator and the TriPlus sampler from the control interface. 7. Remove the actuator body and the ground wire fixing screw. Remove the two screws that fix the actuator body to the fixing arm of the OC head.
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Chapter 5 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector Direct Narrow-Bore 8. Move vertically the valve lever to allows its extraction through the slot on the actuator shaft. Carefully lift up the automatic actuator to remove it from the OC housing. Loosen the two screws A on the side of the OC head.
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Chapter 5 Maintaining a Cold On-Column Injector Direct Narrow-Bore Replace the Rotary Valve Seal 10. Unscrew the two Allen bolts that fix the injector body to the injector base. Remove the injector body from its base. CAUTION Pay attention not to lose the small needle guide when removing the injector body.
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Chapter 5 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector Direct Narrow-Bore 12. Remove the clip that retains the rotary valve. 13. Push the rotary valve out from the injector head. 14. Push the PTFE seal upwards to eject it. CAUTION In order to avoid leaks of sample from the valve...
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Chapter 5 Maintaining a Cold On-Column Injector Direct Narrow-Bore Replace the Rotary Valve Seal 18. Reassemble the two parts of the injector body. 19. Remount the injector body on its base, tightening the two Allen screws. CAUTION Be careful to reinstall the needle guide with the small cut downwards, otherwise no flow of carrier gas to the column will...
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Chapter 5 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector Direct Narrow-Bore 20. . Fix the OC head on the ceiling of the GC and tighten the two screws A on the side of the OC head previously loosened. 21.
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Chapter 5 Maintaining a Cold On-Column Injector Direct Narrow-Bore Replace the Rotary Valve Seal 22. .Adjust the position of the automatic actuator up to align the fixing holes provided on the actuator body with the corresponding fixing holes located on the fixing arm of the OC head. Fix the parts by using the two fixing screws.
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Chapter 5 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector Direct Narrow-Bore 28. Press OVEN, scroll to and press ON. Temp 29. Perform a leak check according to Performing a Leak Check (Capillary Column) Operating Sequence on page 181. From the data system in use, enable the automatic actuator to open and close the rotary valve of the OC injector by using the direct...
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Chapter 5 Maintaining a Cold On-Column Injector Direct Narrow-Bore Replace the Rotary Valve Seal Maintenance and Troubleshooting Manual...
Chapter 6 Maintaining a Cold On-Column Injector Cold On-Column Injector Maintenance Cold On-Column Injector Maintenance This injector will normally be serviced by Thermo Fisher Scientific authorized technical personnel and do not require periodic maintenance, except for septum replacement in the automatic version. The PTFE seal of the rotary valve, if worn, can be replaced by the user.
Chapter 6 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector OPERATING SEQUENCE Replace the Rotary Valve Seal NOTE Drawings refer to the Manual Cold On-Column Injector. Materials needed • 5.5 mm hexagonal wrench • PTFE seal (P/N 290 070 01) •...
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Chapter 6 Maintaining a Cold On-Column Injector Replace the Rotary Valve Seal 5. Loosen the screw that retains the actuation lever of the injector. 6. Remove the lever. 7. Unscrew the two Allen bolts that fix the injector body to the injector base. Remove the injector body from its base.
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Chapter 6 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector 8. Disassemble the injector body, separating the head from the lower part. 9. Remove the clip that retains the rotary valve. 10. Push the rotary valve out from the injector head.
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Chapter 6 Maintaining a Cold On-Column Injector Replace the Rotary Valve Seal 12. Insert a new PTFE seal into its housing, paying attention to the alignment of the holes. 13. Insert the rotary valve into its housing. 14. Fix the rotary valve with the relevant clip. 15.
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Chapter 6 Replace the Rotary Valve Seal Maintaining a Cold On-Column Injector 16. Remount the injector body on its base, tightening the two Allen screws. 17. Insert the valve lever into its housing, tightening the retaining screw. CAUTION Be careful to reinstall the needle guide with the small cut downwards, otherwise no flow of carrier gas to the column will...
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Chapter 6 Maintaining a Cold On-Column Injector Replace the Rotary Valve Seal 20. Press OVEN, scroll to and press ON. Temp 21. Perform a leak check according to Performing a Leak Check (Capillary Column) Operating Sequence on page 181. Maintenance and Troubleshooting Manual...
Chapter 7 Maintaining a Packed Column Injector Packed Column Injector Maintenance Packed Column Injector Maintenance The Packed Column injector and its interface module will normally be serviced by Thermo Fisher Scientific authorized technical personnel. In order to keep the injector operating at peak performance, you should periodically replace the septum.
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Chapter 7 Replacing the Septum Maintaining a Packed Column Injector OPERATING SEQUENCE Replacing the Septum Materials needed • Non metallic sharp tool • Septum (see # 7, Table 7-1 on page 123) • Tweezers CAUTION This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the injector must be cooled to room temperature.
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Chapter 7 Maintaining a Packed Column Injector Replacing the Septum 5. When the inlet reaches the room temperature, RIGHT CARRIER (PKD) press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating. Pressure 30.0 30.0 Col. flow 3.00 < 6.
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Chapter 7 Replacing the Septum Maintaining a Packed Column Injector 9. Insert a new septum in the septum cap. CAUTION Use tweezers to avoid touching the septum with your fingers. 10. Tighten the septum cap. CAUTION Do not overtighten the injector cap.
Chapter 8 Maintaining a Purged Packed Column Injector Purged Packed Column Injector Maintenance Purged Packed Column Injector Maintenance The Purged Packed Column injector and its interface module will normally be serviced by Thermo Fisher Scientific authorized technical personnel. In order to operate at peak performances, the injector requires periodic maintenance from the user.
Chapter 8 Replace the Septum Maintaining a Purged Packed Column Injector OPERATING SEQUENCE Replace the Septum Materials needed • Non metallic sharp tool • Septum (see # 7, Table 8-1 on page 131) • Tweezers WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the injector must be cooled to room temperature.
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Chapter 8 Maintaining a Purged Packed Column Injector Replace the Septum 5. When the inlet reaches the room temperature, RIGHT CARRIER (PPKD) press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating. Pressure 30.0 30.0 Col. flow 3.00 <...
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Chapter 8 Replace the Septum Maintaining a Purged Packed Column Injector 9. Insert a new septum in the septum cap. CAUTION Use tweezers to avoid touching the septum with your fingers. 10. Tighten the septum cap. CAUTION Do not overtighten the injector cap.
Chapter 8 Maintaining a Purged Packed Column Injector Clean or Replace the Liner OPERATING SEQUENCE Clean or Replace the Liner Materials needed • Glass liner (see item 8, Table 5-1) • Ultrasonic bath • Methanol/acetone mixture (1:1) • Tweezers WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the injector must be cooled to room temperature.
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Chapter 8 Clean or Replace the Liner Maintaining a Purged Packed Column Injector 3. Press LEFT INLET or RIGHT INLET depending on RIGHT INLET (PPKD) which injector is operating. In the following example, a PPKD injector installed on the right Temp 200 <...
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Chapter 8 Maintaining a Purged Packed Column Injector Clean or Replace the Liner 9. Unscrew the retaining nut at the bottom of the injector. 10. Remove the liner and the ferrule. 11. Remove the ferrule from the liner. 12. If you are using a new liner, go to step 14. If you are cleaning the liner, put the dirty liner into an ultrasonic bath filled with a methanol/ acetone mixture (1:1) and clean it for about half...
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Chapter 8 Clean or Replace the Liner Maintaining a Purged Packed Column Injector 14. Insert a ferrule on the new (or cleaned) liner, using tweezers to hold it. CAUTION Be careful not to damage the graphite seal or allow graphite to entering the liner.
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Chapter 8 Maintaining a Purged Packed Column Injector Clean or Replace the Liner 20. Press OVEN, scroll to and press ON. Temp 21. Press LEFT INLET or RIGHT INLET, depending on which injector is operating, scroll to Temp press ON. 22.
Maintaining a PTV Injector Chapter at a Glance… PTV Injector .......................142 PTV Injector Maintenance .................144 PTV Troubleshooting ..................171 Operating Sequences Replace the Septum ....................147 Clean or Replace the Liner .................151 Replace a Broken Liner ..................157 Adjust a Quartz Wool Packing ................165 Maintenance and Troubleshooting Manual...
Chapter 9 Maintaining a PTV Injector PTV Injector Maintenance Table 9-1. PTV Injector parts identification table (Continued) Graphite ferrule for 0.2 mm ID column 290 134 89 Graphite ferrule for 0.25 mm ID column 290 134 88 Graphite ferrule for 0.32 mm ID column 290 134 87 Graphite ferrule for 0.53 mm ID column 290 134 86...
Chapter 9 PTV Injector Maintenance Maintaining a PTV Injector It is a good practice to change the septum with a new one every time the liner is replaced or cleaned. The operating sequence suggested for the replacement of the septum is reported on page 147. When cleaning or replacing the liner The liner must be replaced periodically, depending on the number of injections performed and the characteristics of the samples injected.
Chapter 9 Maintaining a PTV Injector PTV Injector Maintenance If a liner breaks inside the injector When replacing or removing a glass liner, it might break inside the injector. In this case the broken parts of the liner must be removed from the injector, including the glass splinters that might fall into the lower part of the vaporization chamber.
Chapter 9 Replace the Septum Maintaining a PTV Injector OPERATING SEQUENCE Replace the Septum Materials needed • Non metallic sharp tool • Septum (P/N 313 132 25) • Tweezers WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the injector must be cooled to room temperature.
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Chapter 9 Maintaining a PTV Injector Replace the Septum 5. When the inlet reaches the room temperature, RIGHT CARRIER (PTV) press RIGHT CARRIER. Pressure 30.0 30.0 and press OFF. 6. Scroll to Pressure Col. flow 3.00 < Lin. Veloc. (60.9) 7.
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Chapter 9 Replace the Septum Maintaining a PTV Injector 9. Remove the septum from the septum holder (use non-metallic tools) 10. Insert a new septum into the septum holder. CAUTION Use tweezers to avoid touching the septum with your fingers. 11.
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Chapter 9 Maintaining a PTV Injector Replace the Septum 16. Press RIGHT INLET, scroll to and press ON. Temp 17. Perform a leak check according to Performing a Leak Check (Capillary Column) Operating Sequence on page 181. Maintenance and Troubleshooting Manual...
Chapter 9 Clean or Replace the Liner Maintaining a PTV Injector OPERATING SEQUENCE Clean or Replace the Liner Materials needed • Screwdriver (P/N 205 026 03) • Liner (see Table 9-2, on page 145) • Graphite seal (P/N 290 134 17) •...
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Chapter 9 Maintaining a PTV Injector Clean or Replace the Liner 3. Press RIGHT INLET. RIGHT INLET (PTV) and press OFF. 4. Scroll to Temp Temp 50 < Pressure Mode split 5. When the inlet reaches the room temperature, RIGHT CARRIER (PTV) press RIGHT CARRIER depending on which Col.
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Chapter 9 Clean or Replace the Liner Maintaining a PTV Injector 9. Use the screwdriver provided with the GC to remove the injector liner cap. 10. Use tweezers to remove the liner with the graphite seal. CAUTION If you are using a glass liner, be careful not to break it inside the injector when removing it.
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Chapter 9 Maintaining a PTV Injector Clean or Replace the Liner 12. Using tweezers, remove the liner from the bath and dry it with compressed clean air. PRECAUTIONS 13. Holding the new (or cleaned) liner with tweezers, place a graphite seal over the liner, making sure to leave a distance of about 10 mm between the seal and the liner end.
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Chapter 9 Clean or Replace the Liner Maintaining a PTV Injector 15. Tighten the liner cap using the screwdriver provided with the GC. 16. Remove the septum from the septum holder using a non-metallic sharp tool. 17. Insert a new septum into the septum holder. CAUTION Use tweezers to avoid touching the septum with your fingers.
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Chapter 9 Maintaining a PTV Injector Clean or Replace the Liner 18. Place the septum support into its housing inside the injector. 19. Reinsert the septum holder with the septum. 20. Tighten the injector cap to finger tight. CAUTION Do not overtighten the injector cap.
Chapter 9 Replace a Broken Liner Maintaining a PTV Injector OPERATING SEQUENCE Replace a Broken Liner Materials needed • Screwdriver (P/N 205 026 03) • Liner removing tool (P/N 398 014 04) • Glass liner (see Table 9-2, on page 145) •...
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Chapter 9 Maintaining a PTV Injector Replace a Broken Liner 5. When the inlet reaches the room temperature, RIGHT CARRIER (PTV) press RIGHT CARRIER. Col. flow < and press OFF. 6. Scroll to Pressure Pressure Flow mode con pres 7. Unscrew the injector cap. 8.
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Chapter 9 Replace a Broken Liner Maintaining a PTV Injector 9. Use the screwdriver provided with the GC to remove the injector liner cap. 10. Use tweezers to remove the upper part of the broken liner (with the graphite seal) from the injector.
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Chapter 9 Maintaining a PTV Injector Replace a Broken Liner 11. Unscrew the nut that retains the analytical column. 12. Remove the analytical column with its ferrule. 13. Inserting the steel thread provided specifically for this purpose, remove the possible glass fragments from the vaporization chamber pushing them out through the upper opening of the injector.
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Chapter 9 Replace a Broken Liner Maintaining a PTV Injector 14. Use tweezers to reinsert the spacer inside the injector, complying with the correct orientation. 15. Holding a liner with tweezers, place a graphite seal over it, making sure to leave a distance of about 10 mm between the seal and the liner end.
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Chapter 9 Maintaining a PTV Injector Replace a Broken Liner 17. Tighten the liner cap using the screwdriver provided with the GC. 18. Insert the analytical column with its ferrule into the bottom of the injector in its previous ™ position.
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Chapter 9 Replace a Broken Liner Maintaining a PTV Injector 20. Remove the septum from the septum holder using a non-metallic sharp tool. 21. Insert a new septum into the septum holder. CAUTION Use tweezers to avoid touching the septum with your fingers. 22.
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Chapter 9 Maintaining a PTV Injector Replace a Broken Liner 24. Tighten the injector cap to finger tight. CAUTION Do not overtighten the injector cap. You could damage the septum and affect performance. 25. Press RIGHT CARRIER, scroll to Pressure press ON.
Chapter 9 Adjust a Quartz Wool Packing Maintaining a PTV Injector OPERATING SEQUENCE Adjust a Quartz Wool Packing Materials needed • Screwdriver (P/N 205 026 03) • Graphite seal (P/N 290 134 17) • Non metallic sharp tool • Thin (<2 mm diameter) non metallic bar (e.g. 1.6 mm PEEK tube) •...
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Chapter 9 Maintaining a PTV Injector Adjust a Quartz Wool Packing 5. When the inlet reaches the room temperature, RIGHT CARRIER (PTV) press RIGHT CARRIER. Col. flow < and press OFF. 6. Scroll to Pressure Pressure Flow mode con pres 7.
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Chapter 9 Adjust a Quartz Wool Packing Maintaining a PTV Injector 9. Use the screwdriver provided with the GC to remove the injector liner cap. 10. Use tweezers to remove the liner with the graphite seal. 11. Remove the graphite seal from the liner. Use tweezers to handle the liner.
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Chapter 9 Maintaining a PTV Injector Adjust a Quartz Wool Packing 12. Insert a thin, non metallic bar into the ends of the liner and push the quartz wool so to have a distance of about 28 mm between the packing and the ends of the liner.
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Chapter 9 Adjust a Quartz Wool Packing Maintaining a PTV Injector 15. Tighten the liner cap using the screwdriver provided with the GC. 16. Remove the septum from the septum holder using a non-metallic sharp tool. 17. Insert a new septum into the septum holder. CAUTION Use tweezers to avoid touching the septum with your fingers.
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Chapter 9 Maintaining a PTV Injector Adjust a Quartz Wool Packing 18. Place the septum support into its housing inside the injector. 19. Reinsert the septum holder with the septum. 20. Tighten the injector cap to finger tight. CAUTION Do not overtighten the injector cap.
Chapter 9 PTV Troubleshooting Maintaining a PTV Injector PTV Troubleshooting Sensitivity Low sensitivity is commonly caused by incorrect operating conditions. It might also be due to a dirty liner or to a liner wrong sized with regards to the volume of the sample injected.
Chapter 9 Maintaining a PTV Injector PTV Troubleshooting Troubleshooting the PTV Injector Table 9-3. PTV Troubleshooting Table Symptom Diagnosis Remedy Transfer temperature too low Set Transfer temp to a higher value. Transfer time too low Set transfer time or cleaning time to a value close to the whole GC run time.
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Chapter 9 PTV Troubleshooting Maintaining a PTV Injector Table 9-3. PTV Troubleshooting Table (Continued) Symptom Diagnosis Remedy Liner not suitable for the Replace the liner with an adequate one. actual sample A lower diameter liner would improve the sample transfer. Refer to Clean or Replace the Liner Operating Sequence...
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Chapter 9 Maintaining a PTV Injector PTV Troubleshooting Table 9-3. PTV Troubleshooting Table (Continued) Symptom Diagnosis Remedy Transfer temperature too low Set Transfer temp to a higher value. Transfer time too low Set transfer time or cleaning time to a value close to the whole GC run time.
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Chapter 9 PTV Troubleshooting Maintaining a PTV Injector Table 9-3. PTV Troubleshooting Table (Continued) Symptom Diagnosis Remedy Liner diameter too large Replace the liner with one of smaller diameter to improve transfer efficiency. Refer to Clean or Replace the Liner Operating Sequence on page 151.
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Chapter 9 Maintaining a PTV Injector PTV Troubleshooting Table 9-4. PTVLV Troubleshooting Table Symptom Diagnosis Remedy Transfer temperature too low Set Transfer temp to a higher value. Transfer time too low Set transfer time or cleaning time to a value close to the whole GC run time.
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Chapter 9 PTV Troubleshooting Maintaining a PTV Injector Table 9-4. PTVLV Troubleshooting Table (Continued) Symptom Diagnosis Remedy Cathalytic degradation of Use an empty deactivated liner reducing sensitive compounds caused the volume injected. Refer to Clean or by the quartz wool Replace the Liner Operating Sequence on page 151.
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Chapter 9 Maintaining a PTV Injector PTV Troubleshooting Maintenance and Troubleshooting Manual...
Ensuring Tightness Chapter at a Glance… Keeping Leaks under Control................180 Operating Sequences Performing a Leak Check (Capillary Column) ..........181 Performing a Leaks Check (Capillary/Packed/UFM Columns)......185 Leak Test the Lines from the Gas Source to the GC ..........188 Maintenance and Troubleshooting Manual...
DCC-equipped systems TRACE GC Ultra, equipped with a DCC (Digital Carrier Control) module features a new user interface menu which guides the user through a sequence of operations necessary to correctly keep under control the pneumatic conditions of the GC system.
Col. Evaluation Figure 10-1. Column-flow Meter Connector Materials needed: • Leak detector (Thermo Scientific GLD Pro, or equivalent) • Column-flow meter connector The column-flow meter connector features two dedicated channels: — A blind channel used to seal the column end when a leak check is ...
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Chapter 10 Ensuring Tightness Performing a Leak Check (Capillary Column) Figure 10-2. Leak Check 3. Press LEAK CHECK to enter Leak Check menu. The displayed options ) depend on the configuration of your GC. Right column Left column In the example, the left column is considered. LEAK CHECK COLUMN Right column Left column...
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Chapter 10 Performing a Leak Check (Capillary Column) Ensuring Tightness 6. In Check at press line set the pressure (pressurization value) at which the leak check must be performed. The range is comprised from 10 to 999 kPa (1.45-145 psi). 7.
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Chapter 10 Ensuring Tightness Performing a Leak Check (Capillary Column) 11. If leaks are detected, check the accessible, critical connections with an electronic leak detector to locate the possible leaks. 12. Eliminate the leaks and repeat the leack check procedure. 13.
• 6MB blind nut (for ECD) • Leak detector (Thermo Scientific GLD Pro, or equivalent) 1. In case the column is already installed, cool down the injector and the detector base body to room temperature. 2. Only for FID, NPD, FPD: remove the detector. Do not remove ECD detector.
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Chapter 10 Ensuring Tightness Performing a Leaks Check (Capillary/Packed/UFM Columns) 1. This item appears if the relevant channel is present and configured. 8. Scroll to the channel of interest and press ENTER to open the following menu: L. COL. LEAK CHECK Start Leak Check Leak Check Settings 9.
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Chapter 10 Performing a Leaks Check (Capillary/Packed/UFM Columns) Ensuring Tightness NOTE To abort Leak Check, press STOP. A relevant message will be displayed. 14. The system is pressurized for one minute, then the pressure value of the carrier is automatically set to Off. The system monitories the pressure for one minute.
5% in 10 minutes. If the value drops down immediately, one or more leaks are present. In this case: 4. Check the connections with the Thermo Scientific GLD Pro leak detector, or equivalent handheld electronic leak detector, to find possible leaks.
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Chapter 10 Leak Test the Lines from the Gas Source to the GC Ensuring Tightness GC 2 GC 3 Cut-off Valve Pressure Gauge GC 1 1/8" Tee with Teflon Tape to Seal Pipe Threads Figure 10-3. Testing Multiple Systems Maintenance and Troubleshooting Manual...
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Chapter 10 Ensuring Tightness Leak Test the Lines from the Gas Source to the GC Maintenance and Troubleshooting Manual...
Maintaining a FID Chapter at a Glance… Flame Ionization Detector (FID) ................192 FID Maintenance ....................194 FID Troubleshooting ..................214 Operating Sequences Clean the Jet .......................195 Replace the Jet....................199 Clean the Collecting Electrode................202 Replace the Collecting Electrode ...............207 Replace the Ignition Assembly................211 Maintenance and Troubleshooting Manual...
Chapter 11 Maintaining a FID FID Maintenance FID Maintenance To ensure optimum performance of the FID, you must keep it clean and free of dust and deposits. Symptoms such as reduced sensitivity and increased noise indicate that detector needs cleaning. To properly maintain the FID, you should perform the following cleaning or replacement sequences: •...
Chapter 11 Clean the Jet Maintaining a FID OPERATING SEQUENCE Clean the Jet Materials needed: • Screwdriver • Tool for extracting the jet (P/N 205 019 00) • Forceps or tweezers • Distiller water • Clean compressed air • GC-grade methanol •...
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Chapter 11 Maintaining a FID Clean the Jet Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DETECTOR (FID) depending on the location of the FID detector, to access the FID control table. In the following Flame Off < example, a FID installed on the right channel is Base temp considered.
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Chapter 11 Clean the Jet Maintaining a FID 6. Using the tool provided with the GC, unscrew the jet. 7. Mechanically remove any contaminating material and sweep with clean compressed air if necessary. 8. Handling the jet with forceps or tweezers, rinse the jet with distilled water, then with methanol.
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Chapter 11 Maintaining a FID Clean the Jet 11. Place the detector cell on the detector base body and tighten the fixing screw. 12. Reconnect the signal and ignition cables to the detector. 13. Reset the detector to the required operating conditions.
Chapter 11 Replace the Jet Maintaining a FID OPERATING SEQUENCE Replace the Jet Materials needed • Screwdriver • Tool for removing the jet (P/N 205 019 00) • Forceps or tweezers • Jet for FID (P/N 404 043 01) WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the detector must be cooled to room temperature.
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Chapter 11 Maintaining a FID Replace the Jet 4. Disconnect the signal and ignition cables from the detector. 5. Loosen the fixing nut on the front of the detector cell and remove it. 6. Using the tool provided with the GC, unscrew the worn jet from the detector base body.
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Chapter 11 Replace the Jet Maintaining a FID 7. Place a new jet into the housing and tighten it with the proper tool. Ensure the jet is perfectly vertically aligned to avoid damaging its ceramic part. 8. Place the detector cell on the detector base body and tighten the fixing screw on the front of the detector cell.
Chapter 11 Maintaining a FID Clean the Collecting Electrode OPERATING SEQUENCE Clean the Collecting Electrode Materials needed • Screwdriver • Pliers • Forceps or tweezers • Ultrasonic cleaning bath • Liquid detergent • Clean compressed air • GC-grade methanol • Clean paper towel WARNING! This operation must be carried out at low temperature to avoid burns.
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Chapter 11 Clean the Collecting Electrode Maintaining a FID Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DETECTOR (FID) depending on the location of the FID detector, to access the FID control table. In the following Flame Off < example, a FID installed on the right channel is Base temp considered.
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Chapter 11 Maintaining a FID Clean the Collecting Electrode 7. Remove the holder assembly of the signal cable by unscrewing the two screws that fix it on the detector cell. 8. Using forceps, unscrew and remove the gold contact pin. 9.
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Chapter 11 Clean the Collecting Electrode Maintaining a FID 13. When the electrode is dry, place it in its housing. Ensure the insert hole is perfectly vertically aligned with the hole on the cell. 14. Using forceps, reconnect the gold contact pin. 15.
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Chapter 11 Maintaining a FID Clean the Collecting Electrode 16. Screw the detector cap into its housing. 17. Place the detector cell on the base body and tighten the fixing screw. 18. Reconnect the signal and ignition cables to the detector.
Chapter 11 Replace the Collecting Electrode Maintaining a FID OPERATING SEQUENCE Replace the Collecting Electrode Materials needed • Screwdriver • Pliers • Forceps or tweezers • Collecting electrode (P/N 259 011 15) WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the detector must be cooled to room temperature.
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Chapter 11 Maintaining a FID Replace the Collecting Electrode 4. Disconnect the signal and ignition cables from the detector. 5. Loosen the fixing nut on the front of the detector cell and remove it. 6. Unscrew and remove the cap of the detector cell.
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Chapter 11 Replace the Collecting Electrode Maintaining a FID 10. Place the new collecting electrode into its housing. Ensure the insert hole is perfectly vertically aligned with the hole on the cell. 11. Using forceps, reconnect the gold contact pin. 12.
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Chapter 11 Maintaining a FID Replace the Collecting Electrode 13. Screw the detector cap into its housing. 14. Place the detector cell on its base body and tighten the fixing screw. 15. Reconnect the signal and ignition cables to the detector.
Chapter 11 Replace the Ignition Assembly Maintaining a FID OPERATING SEQUENCE Replace the Ignition Assembly Material needed: • Screwdriver • Connector Holder Assembly (P/N 206 016 03) WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the detector must be cooled to room temperature.
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Chapter 11 Maintaining a FID Replace the Ignition Assembly 4. Disconnect the signal and ignition cables form the detector. 5. Loosen the fixing nut on the front of the detector cell and remove it. 6. Unscrew the two fixing screws and remove the lower connector holder assembly from the detector cell.
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Chapter 11 Replace the Ignition Assembly Maintaining a FID 7. Remount the new connector holder assembly and fix it to the detector cell using the two screws. Make sure the connecting fork is placed downwards to achieve the correct contact with the jet.
Chapter 11 Maintaining a FID FID Troubleshooting FID Troubleshooting Change in Sensitivity The sensitivity of the Flame Ionization Detector depends on the carrier and detector gases flow rates and to the detector temperature. The gas flow rates must be set correctly for proper FID operation. Gases The gases normally used with FID are reported in Table 11-2.
Chapter 11 FID Troubleshooting Maintaining a FID The FID sensitivity will be reduced as hydrogen flow rate is above or below the optimal value. The flow rate of the air is less critical than the hydrogen one. An excessive amount of air will destabilize the flame, causing noise and eventual flameout.
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Operating cracked flame Sequence on page 199 for instructions. Check for a blocked jet by measuring the hydrogen flow with the Thermo Scientific GFM Pro Flowmeter (or equivalent). Blocked jet tip If required, remove and clean the jet following the...
Chapter 11 FID Troubleshooting Maintaining a FID Contamination All organic compounds that pass through the FID are burnt in the flame. Some compounds can produce detector contamination, resulting in a high noise baseline. If this symptom is found, clean the collecting electrode. Refer to the Clean the Collecting Electrode Operating Sequence on page 202 for instructions.
Maintaining an Electron Capture Detector Chapter at a Glance… Electron Capture Detector (ECD) ..............220 ECD Maintenance ....................222 Wipe Test ......................223 Troubleshooting..................235 Operating Sequences Clean the Collecting Electrode................226 Replace the Collecting Electrode ...............229 Replace the Silver Seal..................232 Maintenance and Troubleshooting Manual...
Chapter 12 Maintaining an Electron Capture Detector Electron Capture Detector (ECD) Electron Capture Detector (ECD) Maintenance and Troubleshooting Manual...
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Chapter 12 Electron Capture Detector (ECD) Maintaining an Electron Capture Detector Table 12-1. Electron Capture Detector (ECD) parts identification table Description Detector cell Fixing nut Chimney Excitation connector Signal connector Detector cover Collecting electrode 277 003 50 Silver seal 290 150 58 Temperature sensor/heater assembly 190 500 87 ECD fixing tool...
Chapter 12 Maintaining an Electron Capture Detector ECD Maintenance ECD Maintenance The ECD, if properly used, has a good resistance against contamination thanks to its unique internal geometry. However, some critical operating conditions may give rise, in the long run, to contamination of the collecting electrode. This contamination is highlighted by an excessive increase of the base frequency and a baseline drift when the reference current or the pulse amplitude is changed.
Chapter 12 Wipe Test Maintaining an Electron Capture Detector Wipe Test Before leaving the factory, each ECD is leak tested for surface radio contamination by means of the Wipe Test method. Each detector is provided with a Wipe Test Certificate reporting the results of the values found and the procedure followed.
Chapter 12 Maintaining an Electron Capture Detector Wipe Test Wipe Test Certificate Certificate number Wipe test date Source Serial Number Radionuclide Detector Model Detector Serial Number ASSAY RESULTS* Observed Counting Rate Radionuclide Counting Background c.p.m. net d.p.m. (**) Activity Bq Efficiency c.p.m (**)
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Chapter 12 Wipe Test Maintaining an Electron Capture Detector ECD Wipe Test is to be carried out under a controlled procedure as reported below: Procedure Wet cotton wool swab with methanol. Wipe the outer surface of the ECD. Remove metal exit tube from top of ECD. Wipe the bottom of the exit tube.
Chapter 12 Maintaining an Electron Capture Detector Clean the Collecting Electrode OPERATING SEQUENCE Clean the Collecting Electrode Materials needed • Screwdriver • 2.5 mm Allen wrench • Tweezers • Ultrasonic cleaning bath • GC-grade hexane • GC-grade toluene • Fine emery paper WARNING! Any maintenance or repair operations involving the radioactive source must be performed ONLY by qualified personnel duly authorized to handle radioactive material.
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Chapter 12 Clean the Collecting Electrode Maintaining an Electron Capture Detector 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DETECTOR (ECD) depending on the location of the ECD, to access the ECD control table. In the following Base temp Off < example, an ECD installed on the right channel ECD temp is considered.
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Chapter 12 Maintaining an Electron Capture Detector Clean the Collecting Electrode 8. Remount the electrode without touching it. Use tweezers. 9. Remount the detector cover with the chimney. 10. Reconnect the signal and ignition cables to the detector. 11. Reset the detector to the required operating conditions.
Chapter 12 Replace the Collecting Electrode Maintaining an Electron Capture Detector OPERATING SEQUENCE Replace the Collecting Electrode Materials needed • Screwdriver • 2.5 mm Allen wrench • Tweezers • Collecting Electrode (P/N 277 003 50) WARNING! Any maintenance or repair operations involving the radioactive source must be performed ONLY by qualified personnel duly authorized to handle radioactive material.
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Chapter 12 Maintaining an Electron Capture Detector Replace the Collecting Electrode 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DETECTOR (ECD) depending on the location of the ECD, to access the ECD control table. In the following Base temp Off < example, an ECD installed on the right channel ECD temp is considered.
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Chapter 12 Replace the Collecting Electrode Maintaining an Electron Capture Detector 7. Using tweezers, replace the collecting electrode with a new one and tighten it. 8. Remount the cover with the chimney on the detector. 9. Reconnect the signal and ignition cables to the detector.
Chapter 12 Maintaining an Electron Capture Detector Replace the Silver Seal OPERATING SEQUENCE Replace the Silver Seal Materials needed • Silver seal (P/N 290 150 58) • ECD fixing tool (P/N 205 021 50) • Tweezers WARNING! Any maintenance or repair operations involving the radioactive source must be performed ONLY by qualified personnel duly authorized to handle radioactive material.
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Chapter 12 Replace the Silver Seal Maintaining an Electron Capture Detector 4. Disconnect the signal, excitation and heater cables from the detector. 5. Loosen the nut that fixes the detector to its base body with the proper tool contained in the standard outfit.
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Chapter 12 Maintaining an Electron Capture Detector Replace the Silver Seal 8. Insert a new silver seal on the lower part of the ECD detector. 9. Remount the detector on its base body, tightening the fixing nut with the proper tool. 10.
Chapter 12 ECD Troubleshooting Maintaining an Electron Capture Detector ECD Troubleshooting Change in Sensitivity Temperature The effect of a temperature change on the ECD response generally depends on the compounds analyzed. Gases The ECD behavior can be affected by a change of the total flow of the gases through the cell.
Chapter 12 Maintaining an Electron Capture Detector ECD Troubleshooting NOTE When packed columns are used, the make-up gas (as carrier gas type) is used only if strictly required. WARNING! It is the customer’s responsibility to ensure compliance with all local safety regulations concerning gas supplies.
Chapter 12 ECD Troubleshooting Maintaining an Electron Capture Detector Troubleshooting the ECD Table 12-3. ECD Troubleshooting Table Symptom Diagnosis Remedy Impure gas supply. Use high purity grade gases and filters to trap moisture and oxygen. No (or insufficient) flow of Increase make-up gas flow rate.
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Chapter 12 Maintaining an Electron Capture Detector ECD Troubleshooting Table 12-3. ECD Troubleshooting Table (Continued) Symptom Diagnosis Remedy Contaminated collecting electrode Refer to the notes reported in the ECD Maintenance paragraph on page 222. Contact your customer support Negative dips after organization.
Maintaining a Nitrogen Phosphorus Detector Chapter at a Glance… Nitrogen Phosphorus Detector (NPD)..............240 NPD Maintenance ....................242 Troubleshooting..................264 Operating Sequences Clean the Jet .......................243 Replace the Jet....................247 Clean the Collecting Electrode................251 Replace the Collecting Electrode ...............256 Replace the NPD Thermionic Source..............260 Maintenance and Troubleshooting Manual...
Chapter 13 Maintaining a Nitrogen Phosphorus Detector NPD Maintenance NPD Maintenance To ensure optimum performance of the NPD, you must keep it clean and free of dust and deposits. Symptoms such as reduced sensitivity and increased noise indicate that detector cleaning or thermionic source replacement could be necessary.
Chapter 13 Clean the Jet Maintaining a Nitrogen Phosphorus Detector OPERATING SEQUENCE Clean the Jet Materials needed • Screwdriver • Tool for extracting the jet (P/N 205 019 00) • Forceps or tweezers • Ultrasonic cleaning bath • Liquid detergent •...
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Chapter 13 Maintaining a Nitrogen Phosphorus Detector Clean the Jet 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DETECTOR (NPD) depending on the location of the NPD detector, to access the NPD control table. In the Source cur,A Off < following example, a NPD installed on the right Base temp channel is considered.
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Chapter 13 Clean the Jet Maintaining a Nitrogen Phosphorus Detector 6. Using the tool provided with the GC, unscrew the metal jet. 7. Place the jet in the ultrasonic bath filled with liquid detergent and clean it for about five minutes.
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Chapter 13 Maintaining a Nitrogen Phosphorus Detector Clean the Jet 10. Place the jet into its housing and tighten it with the proper tool. 11. Place the detector cell on the detector base body and reconnect the fixing screw on the front of the detector cell.
Chapter 13 Replace the Jet Maintaining a Nitrogen Phosphorus Detector OPERATING SEQUENCE Replace the Jet Materials needed • Screwdriver • Tool for extracting the jet (P/N 205 019 00) • Forceps or tweezers • Metal jet for NPD (P/N 404 043 02) WARNING! This operation must be carried out at low temperature to avoid burns.
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Chapter 13 Maintaining a Nitrogen Phosphorus Detector Replace the Jet 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DETECTOR (NPD) depending on the location of the NPD detector, to access the NPD control table. In the Source cur,A Off < following example, a NPD installed on the right Base temp channel is considered.
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Chapter 13 Replace the Jet Maintaining a Nitrogen Phosphorus Detector 6. Using the tool provided with the GC, unscrew the worn jet from the detector base body. 7. Place a new jet into its housing and tighten it with the proper tool. Maintenance and Troubleshooting Manual...
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Chapter 13 Maintaining a Nitrogen Phosphorus Detector Replace the Jet 8. Reinsert the detector cell on the detector base body and tighten the fixing screw. 9. Reconnect the signal and ignition cables to the detector. 10. Reset the detector to the required operating conditions.
Chapter 13 Clean the Collecting Electrode Maintaining a Nitrogen Phosphorus Detector OPERATING SEQUENCE Clean the Collecting Electrode Materials needed • Screwdriver • Pliers • Forceps or tweezers • Ultrasonic cleaning bath • Liquid detergent • Clean compressed air • GC-grade methanol •...
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Chapter 13 Maintaining a Nitrogen Phosphorus Detector Clean the Collecting Electrode 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DETECTOR (NPD) depending on the location of the NPD detector, to access the NPD control table. In the Source cur,A Off < following example, a NPD installed on the right Base temp channel is considered.
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Chapter 13 Clean the Collecting Electrode Maintaining a Nitrogen Phosphorus Detector 7. Remove the holder assembly of the signal cable by unscrewing the two screws that fix it on the detector cell. 8. Using forceps, unscrew and remove the contact pin.
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Chapter 13 Maintaining a Nitrogen Phosphorus Detector Clean the Collecting Electrode 13. Place the collecting electrode into its housing. Ensure the insert hole is perfectly vertically aligned to the hole present on the cell. 14. Using forceps, reconnect the gold contact pin. 15.
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Chapter 13 Clean the Collecting Electrode Maintaining a Nitrogen Phosphorus Detector 16. Place the detector cell on the detector base body and tighten the fixing screw. 17. Screw the detector cap into its housing. 18. Reconnect the signal and ignition cables to the detector.
Chapter 13 Maintaining a Nitrogen Phosphorus Detector Replace the Collecting Electrode OPERATING SEQUENCE Replace the Collecting Electrode Materials needed • Screwdriver • Pliers • Forceps or tweezers WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the detector must be cooled to room temperature.
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Chapter 13 Replace the Collecting Electrode Maintaining a Nitrogen Phosphorus Detector 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DETECTOR (NPD) depending on the location of the NPD detector, to access the NPD control table. In the Source cur,A Off < following example, a NPD installed on the right Base temp channel is considered.
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Chapter 13 Maintaining a Nitrogen Phosphorus Detector Replace the Collecting Electrode 7. Remove the holder assembly of the signal cable by unscrewing the two screws that fix it on the detector cell. 8. Using forceps, unscrew and remove the contact pin.
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Chapter 13 Replace the Collecting Electrode Maintaining a Nitrogen Phosphorus Detector 11. Using forceps, reconnect the gold contact pin. 12. Remount the connector holder assembly verifying the contact efficiency. 13. Place the detector cell on the detector base body and tighten the fixing screw. 14.
Chapter 13 Maintaining a Nitrogen Phosphorus Detector Replace the NPD Thermionic Source OPERATING SEQUENCE Replace the NPD Thermionic Source Materials needed: • Screwdriver • 1 mm Allen wrench • Thermionic Source TS-1 (P/N 465 002 50) or TS-2 (P/N 465 002 55) CAUTION Thermionic sources are fragile.
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Chapter 13 Replace the NPD Thermionic Source Maintaining a Nitrogen Phosphorus Detector 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DETECTOR (NPD) depending on the location of the NPD detector, to access the NPD control table. In the Source cur,A Off <...
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Chapter 13 Maintaining a Nitrogen Phosphorus Detector Replace the NPD Thermionic Source 6. Unscrew the grub screw on the collar of the source holder. 7. Remove the four retaining screws of the source metallic socket and pull out the source. 8.
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Chapter 13 Replace the NPD Thermionic Source Maintaining a Nitrogen Phosphorus Detector 10. Place the detector cell on the detector base body and tighten the fixing screw. 11. Reconnect the signal and ignition cables to the detector. 12. Reset the detector to the required operating conditions.
Chapter 13 Maintaining a Nitrogen Phosphorus Detector NPD Troubleshooting NPD Troubleshooting Sensitivity The main cause of changes in sensitivity is related to the Thermionic source. Its gradual depletion results in a drop of sensitivity, that can be compensated by increasing the source current. Take into account that increasing current results in a shorter source life....
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Chapter 13 NPD Troubleshooting Maintaining a Nitrogen Phosphorus Detector Typical flow rates for detector gases are reported in Table 13-3. Table 13-3. Typical NPD operating conditions Flow rate Hydrogen 2-4 mL/min 40-80 mL/min Make-up 10-20 mL/min Maintenance and Troubleshooting Manual...
Chapter 13 Maintaining a Nitrogen Phosphorus Detector NPD Troubleshooting Troubleshooting the NPD Table 13-4. NPD Troubleshooting Table Symptom Diagnosis Remedy Source heating current too low. Increase the heating current. No hydrogen flow. Turn the hydrogen flow on and set it to a correct value. No detector response No air flow.
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Chapter 13 NPD Troubleshooting Maintaining a Nitrogen Phosphorus Detector Table 13-4. NPD Troubleshooting Table (Continued) Symptom Diagnosis Remedy Large negative baseline upset Heating current too low. Slightly increase the source at solvent elution with no heating current. recovery to the original baseline (“Solvent quenching effect”) Background current level too...
Maintaining a Flame Photometric Detector Chapter at a Glance… Flame Photometric Detector (FPD)..............270 FPD Maintenance ....................272 FPD Troubleshooting ..................310 Operating Sequences Clean the Jet .......................273 Clean the Interferential Filter ................278 Clean the Mirror Metal Plug................282 Clean the Flame-side Heat Shield ..............287 Replace the Jet....................292...
Chapter 14 Maintaining a Flame Photometric Detector FPD Maintenance FPD Maintenance To ensure optimum performance of the FPD, you must keep it clean and free of dust and deposits. Symptoms such as reduced sensitivity and increased noise indicate that detector needs cleaning. To properly maintain the FPD, you should perform the following cleaning or replacement sequences: •...
Chapter 14 Clean the Jet Maintaining a Flame Photometric Detector OPERATING SEQUENCE Clean the Jet Materials needed: • Detector fixing tool (P/N 205 021 50) • 5 mm wrench • Forceps or tweezers • Ultrasonic cleaning bath • Liquid detergent •...
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Chapter 14 Maintaining a Flame Photometric Detector Clean the Jet 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DET (FPD) depending on the location of the FPD detector, to access the FPD control table. In the Flame Off < following example, a FPD installed on the right Base temp channel is considered.
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Chapter 14 Clean the Jet Maintaining a Flame Photometric Detector 6. Using the tool provided with the GC, loosen the fixing nut on the base of the detector and remove it. CAUTION Pay attention not to lose the aluminium ring inserted between the detector head and the base body.
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Chapter 14 Maintaining a Flame Photometric Detector Clean the Jet 11. When the jet is dry, insert the jet into the detector base body and tighten it. 12. Place the detector on its base body, paying attention that the aluminium ring has been inserted in the correct position, then tighten the fixing nut.
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Chapter 14 Clean the Jet Maintaining a Flame Photometric Detector 13. Reconnect the signal, excitation voltage and ignition/heating cables to the detector. 14. Switch on the GC power supply and set the detector to the required operating conditions. Refer to the TRACE GC Ultra Operating manual for more information.
Chapter 14 Maintaining a Flame Photometric Detector Clean the Interferential Filter OPERATING SEQUENCE Clean the Interferential Filter Materials needed • Detector fixing tool (P/N 205 021 50) • Paper towels • GC-grade methanol WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the detector must be cooled to room temperature.
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Chapter 14 Clean the Interferential Filter Maintaining a Flame Photometric Detector 4. Switch off the GC power supply. WARNING! Before disconnecting the cables or disassembling the detector, switching off the GC power supply is indispensable to avoid electrical shocks and damages to the instrument.
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Chapter 14 Maintaining a Flame Photometric Detector Clean the Interferential Filter 6. Loosen the knurled nut that fixes the photomultiplier tube and remove it from the detector body. CAUTION The photomultiplier tube could damage if exposed to ambient light with the excitation voltage .
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Chapter 14 Clean the Interferential Filter Maintaining a Flame Photometric Detector 9. Insert the cleansed filter into its housing. The mirror face must be oriented towards the flame. 10. Reassembly the photomultiplier tube and the detector body, then fix them together tightening the knurled nut.
Chapter 14 Maintaining a Flame Photometric Detector Clean the Mirror Metal Plug OPERATING SEQUENCE Clean the Mirror Metal Plug Materials needed • Detector fixing tool (P/N 205 021 50) • 1 mm Allen wrench • Paper towels • Methylene chloride or methanol WARNING! This operation must be carried out at low temperature to avoid burns.
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Chapter 14 Clean the Mirror Metal Plug Maintaining a Flame Photometric Detector 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DET (FPD) depending on the location of the FPD detector, to access the FPD control table. In the Flame Off < following example, a FPD installed on the right Base temp channel is considered.
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Chapter 14 Maintaining a Flame Photometric Detector Clean the Mirror Metal Plug 6. Using the tool provided with the GC, loosen the fixing nut on the base of the detector and remove it. CAUTION Pay attention not to lose the aluminium ring inserted between the detector head and the base body.
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Chapter 14 Clean the Mirror Metal Plug Maintaining a Flame Photometric Detector 9. Insert the mirror plug in the detector body and fix it with the relevant Allen screws. NOTE Before reinserting the plug, inspect the graphite seal inside the plug’s housing.
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Chapter 14 Maintaining a Flame Photometric Detector Clean the Mirror Metal Plug 11. Reconnect the signal, excitation voltage and ignition/heating cables to the detector. 12. Switch on the GC power supply and set the detector to the required operating conditions. Refer to the TRACE GC Ultra Operating manual for more information.
Chapter 14 Clean the Flame-side Heat Shield Maintaining a Flame Photometric Detector OPERATING SEQUENCE Clean the Flame-side Heat Shield Materials needed • Detector fixing tool (P/N 205 021 50) • 1 mm Allen wrench • Cotton sticks • Paper towels •...
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Chapter 14 Maintaining a Flame Photometric Detector Clean the Flame-side Heat Shield 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DET (FPD) depending on the location of the FPD detector, to access the FPD control table. In the Flame Off < following example, a FPD installed on the right Base temp channel is considered.
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Chapter 14 Clean the Flame-side Heat Shield Maintaining a Flame Photometric Detector 6. Using the tool provided with the GC, loosen the fixing nut on the base of the detector and remove it. CAUTION Pay attention not to lose the aluminium ring inserted between the detector head and the base body.
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Chapter 14 Maintaining a Flame Photometric Detector Clean the Flame-side Heat Shield 10. Insert the mirror plug in the detector body and fix it with the relevant Allen screws. NOTE Before reinserting the plug, inspect the graphite seal inside the plug’s housing.
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Chapter 14 Clean the Flame-side Heat Shield Maintaining a Flame Photometric Detector 12. Reconnect the signal, excitation voltage and ignition/heating cables to the detector. 13. Switch on the GC power supply and set the detector to the required operating conditions. Refer to the TRACE GC Ultra Operating manual for more information.
Chapter 14 Maintaining a Flame Photometric Detector Replace the Jet OPERATING SEQUENCE Replace the Jet Materials needed • Detector fixing tool (P/N 205 021 50) • 5 mm wrench • Jet for FPD (P/N 404 045 11) WARNING! This operation must be carried out at low temperature to avoid burns. Therefore, before beginning the sequence, the detector must be cooled to room temperature.
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Chapter 14 Replace the Jet Maintaining a Flame Photometric Detector 4. Switch off the GC power supply. WARNING! Before disconnecting the cables or disassembling the detector, switching off the GC power supply is indispensable to avoid electrical shocks and damages to the instrument.
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Chapter 14 Maintaining a Flame Photometric Detector Replace the Jet 6. Using the tool provided with the GC, loosen the fixing nut on the base of the detector and remove it. CAUTION Pay attention not to lose the aluminium ring inserted between the detector head and the base body.
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Chapter 14 Replace the Jet Maintaining a Flame Photometric Detector 8. Place a new jet into the housing and tighten it. 9. Place the detector on its base body, paying attention that the aluminium ring has been inserted in the correct position, then tighten the fixing nut.
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Chapter 14 Maintaining a Flame Photometric Detector Replace the Jet 10. Reconnect the signal, excitation voltage and ignition/heating cables to the detector. 11. Switch on the GC power supply and set the detector to the required operating conditions. Refer to the TRACE GC Ultra Operating manual for more information.
Chapter 14 Replace the Interferential Filter Maintaining a Flame Photometric Detector OPERATING SEQUENCE Replace the Interferential Filter Materials needed • Detector fixing tool (P/N 205 021 50) • Interferential filter (see Table 14-2 for available filters) • Paper towels Table 14-2. Available interferential filters for the FPD detector Target compound Phosphorus...
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Chapter 14 Maintaining a Flame Photometric Detector Replace the Interferential Filter 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DET (FPD) depending on the location of the FPD detector, to access the FPD control table. In the Flame Off < following example, a FPD installed on the right Base temp channel is considered.
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Chapter 14 Replace the Interferential Filter Maintaining a Flame Photometric Detector 6. Loosen the knurled nut that fixes the photomultiplier tube and remove it from the detector body. CAUTION The photomultiplier tube could damage if exposed to ambient light with the excitation voltage set to .
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Chapter 14 Maintaining a Flame Photometric Detector Replace the Interferential Filter 8. Insert the new filter into its housing. The mirror face must be oriented towards the flame. 9. Reassembly the photomultiplier tube and the detector body, then fix them together tightening the knurled nut.
Chapter 14 Replace the Heat Shields Maintaining a Flame Photometric Detector OPERATING SEQUENCE Replace the Heat Shields Materials needed • Detector fixing tool (P/N 205 021 50) • FPD maintenance kit (P/N 190 045 89) • 1 mm Allen wrench •...
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Chapter 14 Maintaining a Flame Photometric Detector Replace the Heat Shields 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DET (FPD) depending on the location of the FPD detector, to access the FPD control table. In the Flame Off < following example, a FPD installed on the right Base temp channel is considered.
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Chapter 14 Replace the Heat Shields Maintaining a Flame Photometric Detector 6. Using the tool provided with the GC, loosen the fixing nut on the base of the detector and remove it. CAUTION Pay attention not to lose the aluminium ring inserted between the detector head and the base body.
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Chapter 14 Maintaining a Flame Photometric Detector Replace the Heat Shields 9. Loosen the three Allen screws that fix the filter support to the flange of the detector body and remove it. 10. Turn down slowly the detector body and let the filter-side heat shield come out from the flange.
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Chapter 14 Replace the Heat Shields Maintaining a Flame Photometric Detector 12. Loosen the Allen screws that fix the mirror plug and remove it. 13. Insert the handle of a screwdriver or other unsharpened tool in the combustion chamber and push the flame-side heat shield and its graphite seal out from its housing.
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Chapter 14 Maintaining a Flame Photometric Detector Replace the Heat Shields Insert the spacer into the flange, letting it stand out for about 5 mm. 17. Insert a new graphite seal on the spacer, pushing it slowly until it touches the flange. 5 mm 18.
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Chapter 14 Replace the Heat Shields Maintaining a Flame Photometric Detector 20. Insert the mirror plug in the detector body and fix it with the relevant Allen screws. NOTE Before reinserting the plug, inspect the graphite seal inside the plug’s housing.
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Chapter 14 Maintaining a Flame Photometric Detector Replace the Heat Shields 23. Reinsert the filter into the support. The mirror face must be oriented towards the flame CAUTION Avoid touching the filter with your fingers. If you see fingertips on the filter, clean it using a clean paper towel and, if needed, GC-grade methanol before remounting.
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Chapter 14 Replace the Heat Shields Maintaining a Flame Photometric Detector 25. Place the detector on its base body, paying attention that the aluminium ring has been inserted in the correct position, then tighten the fixing nut. 26. Reconnect the signal, excitation voltage and ignition/heating cables to the detector.
Chapter 14 Maintaining a Flame Photometric Detector FPD Troubleshooting FPD Troubleshooting Sensitivity The FPD sensitivity is affected by the temperature. The FPD response decreases with an increase in the detector temperature. In addition, the detector response can be severely reduced if a non-sulphur or non-phosphorus compound is partially or fully eluted with the analyte of interest (quenching).
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Chapter 14 FPD Troubleshooting Maintaining a Flame Photometric Detector The following values of flow rate are recommended: Table 14-4. Recommended gas flow rates for FPD Capillary columns Packed columns Carrier 1÷3 mL/min 30÷50 mL/min Hydrogen 85÷100 mL/min 100÷120 mL/min 100÷120 mL/min 110÷135 mL/min The optimum air flow rate should be found experimentally, setting a proper value for the hydrogen and performing some analyses on a standard mixture at different...
Chapter 14 Maintaining a Flame Photometric Detector FPD Troubleshooting Troubleshooting the FPD Table 14-5. FPD troubleshooting table Symptom Diagnosis Remedy Detector conditioning not Increase detector conditioning time completed Air flow rate set too high Reduce air flow rate High standing current Detector not light-tight Tighten the chimney cap and the and noise...
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Chapter 14 FPD Troubleshooting Maintaining a Flame Photometric Detector Table 14-5. FPD troubleshooting table (Continued) Symptom Diagnosis Remedy Low photomultiplier High Voltage Mode Low sensitivity excitation voltage the FPD control table Inadequate hydrogen flow Set the hydrogen flow rate to a proper rate value.
Chapter 15 Maintaining a Photoionization Detector PID Maintenance PID Maintenance The Photoionization Detector requires relatively little maintenance. To properly maintaining the detector, you should perform the following sequences: • UV lamp replacement • Cleaning the UV lamp window The UV Lamp must be replaced when exhausted, faulty or when a different class of compounds is to be analyzed.
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Chapter 15 Replace the UV Lamp Maintaining a Photoionization Detector OPERATING SEQUENCE Replace the UV Lamp Materials needed • UV Lamp (see Table 15-2 on page page 318) • Viton O-ring for UV lamp (P/N 290 203 38) • Cotton gloves WARNING! UV radiation can cause injuries to your eyes.
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Chapter 15 Maintaining a Photoionization Detector Replace the UV Lamp 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DET (PID) depending on the location of the PID detector, to access the PID control table. In the following Lamp Off < example, a PID installed on the right channel is Base temp considered.
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Chapter 15 Replace the UV Lamp Maintaining a Photoionization Detector 4. Remove the lamp with its Viton O-ring from the lamp holder and store it. CAUTION Avoid touching the lamp and particularly the lamp window and the O-ring with your fingers. Use cotton gloves during this operation.
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Chapter 15 Maintaining a Photoionization Detector Replace the UV Lamp 7. Insert the lamp holder into the lamp housing 8. Tighten the two knurled screws to fix the lamp holder to its housing. 9. In the control table RIGHT DETECTOR (PID) scroll subsequently to Mkup Sheath Gas...
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Chapter 15 Clean the Lamp Window Maintaining a Photoionization Detector OPERATING SEQUENCE Clean the Lamp Window Materials needed • Lamp Polishing kit (P/N 190 048 00) • GC-grade methanol or acetone • Paper towels • Cotton gloves WARNING! UV radiation can cause injuries to your eyes. Therefore, before beginning the sequence, make sure the UV lamp has been switched off.
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Chapter 15 Maintaining a Photoionization Detector Clean the Lamp Window 1. Press LEFT DETECTOR or RIGHT DETECTOR, RIGHT DET (PID) depending on the location of the PID detector, to access the PID control table. In the following Lamp Off < example, a PID installed on the right channel is Base temp considered.
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Chapter 15 Clean the Lamp Window Maintaining a Photoionization Detector 4. Remove the lamp with its Viton O-ring from the lamp holder. WARNING! Avoid touching the lamp and particularly the lamp window and the O-ring with your fingers. Use cotton gloves during this operation.
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Chapter 15 Maintaining a Photoionization Detector Clean the Lamp Window 9. Rinse the lamp window with GC-grade methanol or acetone. 10. Wipe the window using a clean paper towel. 11. Air dry the lamp. 12. Insert the Viton O-ring on the lamp, pushing it in until it touches the flange.
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Chapter 15 Clean the Lamp Window Maintaining a Photoionization Detector 14. Insert the lamp holder into the lamp housing. 15. Tighten the two knurled screws to fix the lamp holder to its housing. 16. In the control table RIGHT DETECTOR (PID) scroll subsequently to Mkup Sheath Gas...
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OPERATING SEQUENCE Checking for Leaks Materials needed • Thermo Scientific GLD Pro leak detector (or equivalent) • PID fixing tool (P/N 205 031 00) WARNING! UV radiation can cause injuries to your eyes. Therefore, before beginning the operation, make sure the UV lamp has been switched off.
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Chapter 15 Checking for Leaks Maintaining a Photoionization Detector 3. Press LEFT CARRIER or RIGHT CARRIER XXX CARRIER (XXX) depending on which injector is operating. Col. flow < 4. Scroll to and set Flow mode con pres Pressure 5. Scroll to and set Pressure Flow mode...
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Chapter 15 Maintaining a Photoionization Detector Checking for Leaks Set the carrier pressure to Off. XXX CARRIER (XXX) The actual value should not change more than Pressure 30.0 5% during two or three minutes. If this occur, Col. flow 3.00 <...
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Chapter 15 Checking for Leaks Maintaining a Photoionization Detector 16. If leaks are still detected, loosen the two knurled nuts that fix the lamp holder to the lamp housing. 17. Remove the lamp housing. Maintenance and Troubleshooting Manual...
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Chapter 15 Maintaining a Photoionization Detector Checking for Leaks 18. Remove the heat sink. 19. Tighten the detector cell using the fixing tool provided. 20. Reassemble the detector and repeat the leak test. Maintenance and Troubleshooting Manual...
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Chapter 15 Checking for Leaks Maintaining a Photoionization Detector 21. If leaks are still present, disassemble completely the detector and replace the two seals (#5 and #2 of the exploded view reported on page 316). 22. Reassemble the detector and repeat the leak test to ensure complete tightness.
Chapter 15 Maintaining a Photoionization Detector PID Troubleshooting PID Troubleshooting Sensitivity Lamp The most common cause of loss of sensitivity is condensation of the effluent on the lamp window, resulting in a progressive increase of absorption of the UV. For long life, the window must be cleaned periodically according to the operating sequence described in the Clean the Lamp Window...
Chapter 15 PID Troubleshooting Maintaining a Photoionization Detector Troubleshooting the PID Table 15-3. PID troubleshooting table Symptom Diagnosis Remedy UV Lamp does not light The lamp has not been used until High current mode? immediately for a long time. the lamp lights, the reset to Lamp not installed Install a suitable UV lamp.
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Chapter 15 Maintaining a Photoionization Detector PID Troubleshooting Table 15-3. PID troubleshooting table (Continued) Symptom Diagnosis Remedy Adsorption effects caused by Remove deposits by baking the cell degradation products inside for two hours at 400°C. the cell If the symptom does not disappears, contact your customer support organization.
Chapter 16 Maintaining a Thermal Conductivity Detector Thermal Conductivity Detector (TCD) Thermal Conductivity Detector (TCD) Maintenance and Troubleshooting Manual...
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Chapter 16 Thermal Conductivity Detector (TCD) Maintaining a Thermal Conductivity Detector Table 16-1. Thermal Conductivity Detector (TCD) parts identification table Description Detector insulated box Reference gas line Make-up gas line Reference gas exhaust Carrier + make-up gas exhaust Transfer line heater Column fitting Fixing nut Kit for connecting capillary columns...
Chapter 16 Maintaining a Thermal Conductivity Detector TCD Maintenance TCD Maintenance The TCD detector does not usually need current maintenance. Nevertheless, if you follow a few simple sequences, you will avoid troubles and prolong the detector’s lifetime. Pay a special attention to avoid contamination or damage of the filaments.
Chapter 16 TCD Troubleshooting Maintaining a Thermal Conductivity Detector TCD Troubleshooting Sensitivity Sensitivity is related to the detector temperature (increasing temperature reduce sensitivity) and to the flow rate of the carrier, reference and make-up gas. A gain in sensitivity can be obtained increasing the gap between the temperature of the block and that of the filaments or increasing the filaments voltage.
Chapter 16 Maintaining a Thermal Conductivity Detector TCD Troubleshooting Troubleshooting the TCD Table 16-2. TCD troubleshooting table Symptom Diagnosis Remedy Unstable regulation of the Check the controllers of the carrier, flow rate of the gases reference and make-up gases work well.
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(Constant Voltage, Constant Temperature). Refer to the TRACE GC Ultra Operating Manual for instructions. Thermal conductivity of the Use a different carrier gas. carrier gas is too close to the...
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Chapter 16 Maintaining a Thermal Conductivity Detector TCD Troubleshooting Table 16-2. TCD troubleshooting table (Continued) Symptom Diagnosis Remedy Faulty temperature control Contact your customer support organization. Baseline drift Refer to Appendix B, Customer Communication, for contact information. Oxidized filaments Contact your customer support organization.
Maintaining Detectors in Stack Configuration Chapter at a Glance… ECD adapted for Stack Configuration..............346 Guidelines for Maintenance ................348 Troubleshooting Guidelines ................386 Operating Sequences Clean or Replace the Collecting Electrode (FID on ECD).........349 Clean or Replace the Collecting Electrode (NPD on ECD) .......356 Clean or Replace the Collecting Electrode (FPD on ECD)........363...
Chapter 17 Maintaining Detectors in Stack Configuration Guidelines for Maintenance Guidelines for Maintenance A FID, NPD or FPD detector can be installed on the top of an ECD with the aid of a specially designed adapter (see ECD adapted for Stack Configuration, page 346) to operate as an auxiliary detector.
Chapter 17 Clean or Replace the Collecting Electrode (FID on ECD) Maintaining Detectors in Stack Configuration OPERATING SEQUENCE Clean or Replace the Collecting Electrode (FID on ECD) Materials needed • Screwdriver • 2.5 mm Allen wrench • 3 mm Allen wrench •...
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Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (FID on ECD) Press AUX. AUXILIARY and press ENTER. 2. Scroll to Detector Signal < Detector Temperature Zones Pressure Channel In the table, scroll to AUX DETECTOR (FID) AUX DETECTOR (FID) and press OFF.
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Chapter 17 Clean or Replace the Collecting Electrode (FID on ECD) Maintaining Detectors in Stack Configuration 8. Wait until the detectors temperature is near to ambient, then disconnect the signal and ignition polarization cables from the FID. 9. Loosen the fixing screw on the front of the FID cell and remove it.
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Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (FID on ECD) 10. Disconnect the signal, excitation and heater cables from the ECD detector 11. Remove the heat shield. 12. Remove the heater from the top of the ECD detector unscrewing and removing the 4 mm Allen fixing screw.
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Chapter 17 Clean or Replace the Collecting Electrode (FID on ECD) Maintaining Detectors in Stack Configuration 13. Remove the detector adapter unscrewing the two 3 mm Allen screws. Use a 2.5 mm Allen wrench. 14. Unscrew the collecting electrode and remove it using tweezers.
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Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (FID on ECD) 18. Reinsert the heater on the top of the ECD detector and fix it with its Allen screw. 19. Slip the heat shield onto the heater 20.
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Chapter 17 Clean or Replace the Collecting Electrode (FID on ECD) Maintaining Detectors in Stack Configuration 21. Reconnect the signal and ignition cables to the FID and the signal, excitation and heater cables to the ECD detector. 22. Press LEFT DETECTOR or RIGHT DETECTOR, depending on the location of the ECD, and reset the ECD to the required operating conditions.
Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (NPD on ECD) OPERATING SEQUENCE Clean or Replace the Collecting Electrode (NPD on ECD) Materials needed • Screwdriver • 2.5 mm Allen wrench • 3 mm Allen wrench •...
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Chapter 17 Clean or Replace the Collecting Electrode (NPD on ECD) Maintaining Detectors in Stack Configuration Press AUX. AUXILIARY and press ENTER. 2. Scroll to Detector Signal < Detector Temperature Zones Pressure Channel In the table, scroll to AUX DETECTOR (NPD) AUX DETECTOR (NPD) and press OFF.
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Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (NPD on ECD) 8. Wait until the detectors temperature is near to ambient, then disconnect the signal and ignition polarization cables from the NPD. 9. Loosen the fixing screw on the front of the NPD cell and remove it.
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Chapter 17 Clean or Replace the Collecting Electrode (NPD on ECD) Maintaining Detectors in Stack Configuration 10. Disconnect the signal, excitation and heater cables from the ECD detector 11. Remove the heat shield. 12. Remove the heater from the top of the ECD detector loosening the Allen fixing screw.
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Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (NPD on ECD) 13. Remove the detector adapter unscrewing the two retaining Allen screws. Use a 2.5 mm Allen wrench. 14. Unscrew the collecting electrode and remove it using tweezers.
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Chapter 17 Clean or Replace the Collecting Electrode (NPD on ECD) Maintaining Detectors in Stack Configuration 18. Reinsert the heater on the top of the ECD detector and fix it with its Allen screw. 19. Slip the heat shield onto the heater 20.
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Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (NPD on ECD) 21. Reconnect the signal and ignition cables to the NPD and the signal, excitation and heater cables to the ECD detector. 22. Press LEFT DETECTOR or RIGHT DETECTOR, depending on the location of the ECD, and reset the ECD to the required operating conditions.
Chapter 17 Clean or Replace the Collecting Electrode (FPD on ECD) Maintaining Detectors in Stack Configuration OPERATING SEQUENCE Clean or Replace the Collecting Electrode (FPD on ECD) Materials needed • Screwdriver • 2.5 mm Allen wrench • 3 mm Allen wrench •...
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Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (FPD on ECD) WARNING! Before disconnecting the cables or disassembling an FPD detector, switching off the GC power supply is imperative to avoid electrical shocks and damages to the instrument.
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Chapter 17 Clean or Replace the Collecting Electrode (FPD on ECD) Maintaining Detectors in Stack Configuration 3. Using the tool provided with the GC, loosen the fixing nut on the base of the FPD detector and remove it. CAUTION Pay attention not to lose the aluminium ring inserted between the detector head and the base body.
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Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (FPD on ECD) 5. Remove the detector adapter unscrewing the two retaining Allen screws. Use a 2.5 mm Allen wrench. 6. Unscrew the collecting electrode and remove it using tweezers.
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Chapter 17 Clean or Replace the Collecting Electrode (FPD on ECD) Maintaining Detectors in Stack Configuration 10. Place the FPD detector on the ECD top cover, paying attention that the aluminium ring has been inserted in the correct position, then tighten the fixing nut.
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Chapter 17 Maintaining Detectors in Stack Configuration Clean or Replace the Collecting Electrode (FPD on ECD) 14. Press LEFT DETECTOR or RIGHT DETECTOR, depending on the location of the ECD, and set the ECD to the required operating conditions. 15. Press AUX. and press ENTER.
Chapter 17 Replace the Silver Seal (FID on ECD) Maintaining Detectors in Stack Configuration OPERATING SEQUENCE Replace the Silver Seal (FID on ECD) Materials needed • Silver seal (P/N 290 150 58) • ECD fixing tool (P/N 205 021 50) •...
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Chapter 17 Maintaining Detectors in Stack Configuration Replace the Silver Seal (FID on ECD) In the table, scroll to AUX DETECTOR (FID) AUX DETECTOR (FID) and press OFF. Flame Flame Off < 4. Scroll subsequently to Base temp,H2 Base temp and press OFF.
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Chapter 17 Replace the Silver Seal (FID on ECD) Maintaining Detectors in Stack Configuration 8. Disconnect the signal and ignition polarization cables from the FID. 9. Disconnect the signal, excitation and heater cables from the ECD detector 10. Loosen the nut that fixes the ECD detector to its base body with the proper tool contained in the standard outfit and remove the detectors from the ECD base body.
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Chapter 17 Maintaining Detectors in Stack Configuration Replace the Silver Seal (FID on ECD) 11. Using tweezers, remove the worn silver seal from its housing in the base body. 12. Insert a new silver seal on the lower part of the ECD detector.
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Chapter 17 Replace the Silver Seal (FID on ECD) Maintaining Detectors in Stack Configuration 13. Remount the detector on its base body, tightening the fixing nut with the proper tool. 14. Reconnect the signal, excitation and heater cables to the ECD detector. 15.
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Chapter 17 Maintaining Detectors in Stack Configuration Replace the Silver Seal (FID on ECD) 16. Press LEFT DETECTOR or RIGHT DETECTOR, depending on the location of the ECD, and reset the ECD to the required operating conditions. 17. Press AUX. and press ENTER.
Chapter 17 Replace the Silver Seal (NPD on ECD) Maintaining Detectors in Stack Configuration OPERATING SEQUENCE Replace the Silver Seal (NPD on ECD) Materials needed • Silver seal (P/N 290 150 58) • ECD fixing tool (P/N 205 021 50) •...
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Chapter 17 Maintaining Detectors in Stack Configuration Replace the Silver Seal (NPD on ECD) In the table, scroll to AUX DETECTOR (NPD) AUX DETECTOR (NPD) and press OFF. Base temp Source cur,A 2.740 < 4. Scroll subsequently to Source curr,H2 Base temp and press OFF.
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Chapter 17 Replace the Silver Seal (NPD on ECD) Maintaining Detectors in Stack Configuration 8. Disconnect the signal and ignition polarization cables from the NPD. 9. Disconnect the signal, excitation and heater cables from the ECD detector 10. Loosen the nut that fixes the ECD detector to its base body with the proper tool contained in the standard outfit and remove the detectors from the ECD base body.
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Chapter 17 Maintaining Detectors in Stack Configuration Replace the Silver Seal (NPD on ECD) 11. Using tweezers, remove the worn silver seal from its housing in the base body. 12. Insert a new silver seal on the lower part of the ECD detector.
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Chapter 17 Replace the Silver Seal (NPD on ECD) Maintaining Detectors in Stack Configuration 13. Remount the detector on its base body, tightening the fixing nut with the proper tool. 14. Reconnect the signal, excitation and heater cables to the ECD detector. 15.
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Chapter 17 Maintaining Detectors in Stack Configuration Replace the Silver Seal (NPD on ECD) 16. Press LEFT DETECTOR or RIGHT DETECTOR, depending on the location of the ECD, and reset the ECD to the required operating conditions. 17. Press AUX. and press ENTER.
Chapter 17 Replace the Silver Seal (FPD on ECD) Maintaining Detectors in Stack Configuration OPERATING SEQUENCE Replace the Silver Seal (FPD on ECD) Materials needed • Silver seal (P/N 290 150 58) • ECD fixing tool (P/N 205 021 50) •...
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Chapter 17 Maintaining Detectors in Stack Configuration Replace the Silver Seal (FPD on ECD) 2. Disconnect the signal, excitation voltage and ignition/heating cables from the FPD detector. 3. Disconnect the signal, excitation and heater cables from the ECD detector. 4. Loosen the nut that fixes the ECD detector to its base body with the proper tool contained in the standard outfit and remove the detectors from the ECD base body.
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Chapter 17 Replace the Silver Seal (FPD on ECD) Maintaining Detectors in Stack Configuration 5. Using tweezers, remove the worn silver seal from its housing in the base body. 6. Insert a new silver seal on the lower part of the ECD detector.
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Chapter 17 Maintaining Detectors in Stack Configuration Replace the Silver Seal (FPD on ECD) 7. Remount the detectors on the ECD base body, tightening the fixing nut with the proper tool. 8. Reconnect the signal, excitation and heater cables to the ECD detector. 9.
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Chapter 17 Replace the Silver Seal (FPD on ECD) Maintaining Detectors in Stack Configuration 11. Press LEFT DETECTOR or RIGHT DETECTOR, depending on the location of the ECD, and set the ECD to the required operating conditions. 12. Press AUX. and press ENTER.
Chapter 17 Maintaining Detectors in Stack Configuration Troubleshooting Guidelines Troubleshooting Guidelines Troubleshooting detectors in stack configuration does not differ from what you would do if they would be installed separately. So, in case of troubles, you will find the necessary information in the relevant chapters of this manual. Incorrect installation of the column In case the ECD features an irregular response or no response at all, while the auxiliary detector auxiliary gives a normal response, this can be due to incorrect...
Regenerating Carrier and Split Lines Filters This chapter provides instruction to regenerate the active carbon filters mounting on the carrier gas line and on the split line when S/SL and PTV injectors are present. Operating Sequences To Regenerate Carrier Gas and Split Lines Filters ..........388 Maintenance and Troubleshooting Manual...
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Chapter 18 Regenerating Carrier and Split Lines Filters To Regenerate Carrier Gas and Split Lines Filters OPERATING SEQUENCE To Regenerate Carrier Gas and Split Lines Filters The carrier gas and split lines active carbon filters must be regenerated annually or when ghost peaks are detected during blank analysis.
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Chapter 18 To Regenerate Carrier Gas and Split Lines Filters Regenerating Carrier and Split Lines Filters Figure 1-1. TRACE GC Ultra Top Cover Removing Active Carbon Filter 1. Use the appropriate wrench the loosen each retaining nut. PURGE CARRIER SPLIT 2.1.
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Chapter 18 Regenerating Carrier and Split Lines Filters To Regenerate Carrier Gas and Split Lines Filters 9. Remove the filter from its line. Regenerating the Active Carbon Filter 10. Connect the inlet of the filter to the external nitrogen line by using the proper nut and ferrule.
Analytical Troubleshooting Chapter at a Glance… Troubleshooting problems related to Baseline .......... page 392 Troubleshooting problems related to Peaks ..........page 395 Troubleshooting problems related to Results ........... page 399 Maintenance and Troubleshooting Manual...
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Chapter 19 Analytical Troubleshooting Baseline SYMPTOMS SOURCE Baseline Behavior Characteristics Cause Remedy Accumulation of stationary Replace the end section of the phase column. Carrier gas cylinder Replace the carrier gas cylinder pressure too low to allow Drifting or increase the pressure. control Drifting carrier gas or Check the gas controllers.
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Chapter 19 Baseline Analytical Troubleshooting Behavior Characteristics Cause Remedy Check the oven temperature, ensuring it doesn't exceed the Excessive column column upper limit. stationary phase bleeding Recondition the column. High-standing current Replace the column. Ensure all interconnections and Loose connections screw connections are tight.
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Chapter 19 Analytical Troubleshooting Baseline Behavior Characteristics Cause Remedy Detector temperature higher Reduce the detector temperature than column maximum to the column temperature upper temperature limit. External electrical Attach an AC line monitor and High-frequency Noise interference check purity of the AC supply noise Loose column fittings Tighten fittings accordingly.
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Chapter 19 Peaks Analytical Troubleshooting SYMPTOMS SOURCE Peaks Behavior Characteristics Cause Remedy Reduce the flow to slightly Column flow too high above optimum. Increase the flow to slightly Column flow too low above optimum. Split flow too low in split Increase the flow to 40-50 injection ml/min.
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Chapter 19 Analytical Troubleshooting Peaks Behavior Characteristics Cause Remedy Decrease the injected amount Column or detector and/or analyte concentrations. overloaded Increase the split ratio. Fronting Column temperature too Increase the temperature. Stationary phase too thin Use a thicker-film column. Replace the cylinder or replace Contaminated carrier gas the filter.
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Chapter 19 Peaks Analytical Troubleshooting Behavior Characteristics Cause Remedy Negative Some Symptom can be normal peaks Carrier gas flow too high Reduce the carrier gas flow rate. Combustion gas flow Check the combustion gas flow. incorrect Detector contaminated Bake out or clean the detector. No peaks after solvent peak FID flame extinguished by...
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Chapter 19 Analytical Troubleshooting Peaks Behavior Characteristics Cause Remedy Glass wool or inlet liner Replace with fresh silanized causing activity wool and a clean inlet liner. Inlet temperature too low Increase the inlet temperature Poor or obstructed column Remake the column inlet Tailing Sample peaks connections...
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Chapter 19 Results Analytical Troubleshooting SYMPTOMS SOURCE Results Behavior Characteristics Cause Remedy Concentration not Ensure that the sample compatible with the concentration is suitable for the dynamic range of the detection system. detection system Inappropriate injection Try a different injection technique technique.
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Chapter 19 Analytical Troubleshooting Results Behavior Characteristics Cause Remedy Leaks in the GC carrier gas Run a leak test and correct leaks. line. Poor with normal Syringe leaks during Replace syringe or piston seals, sensitivity retention time injection if applicable. Split injection temperature Increase the temperature of the too low...
Customer Communication Thermo Fisher Scientific provides comprehensive technical assistance worldwide and is dedicated to the quality of our customer relationships and services. This appendix also contains a one-page Reader Survey. Use this survey to give us feedback on this manual and help us improve the quality of our documentation How To Contact Us http://www.thermo.com/com/cda/resources/resource_detail/1,,12512,00.html address for products information.
Appendix A Customer Communication How To Contact Us Reader Survey TRACE™ GC Product: Manual: Maintenance and Troubleshooting Manual Part No.: 31709180 Please help us improve the quality of our documentation by completing and returning this survey. Circle one number for each of the statements below. Strongly Strongly Agree...
Reagents Safety Information Material Safety Data Sheets for the chemicals mentioned in the sequences in this manual should be requested from respective manufacturers. You should comply with the relevant legislation in your area. Chemical safety information is also available from the Internet. For example, International Chemical Safety Cards can be found at http://www.cdc.gov/niosh/ ipcs/ipcsname.html...
Glossary This section contains an alphabetical list and descriptions of terms used in this guide and the help diskette. It also includes abbreviations, acronyms, metric prefixes, and symbols. ampere alternating current analog-to-digital converter byte (8 b) baud rate data transmission speed in events per second ºC Celsius Carriage and Insurance Paid To...
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Glossary Electron Capture Detector electromagnetic compatibility electrostatic discharge ºF Fahrenheit Flame Ionization Detector Free on Board Flame Photometric Detector foot gram gain A measure of the ability of an electronic circuit or device to increase the magnitude of an electronic input parameter. gas chromatograph electrical ground height...
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Glossary high voltage hertz (cycles per second) inside diameter International Electrotechnical Commission impulse transient inch input/output kilo (10 or 1024) Kelvin kilogram kilopascal length liter Local Area Network pound light-emitting diode LVOCI Large Volume On-Column Injector LVSL Large Volume Injector Maintenance and Troubleshooting Manual...
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Glossary meter (or milli [10 mega (10 µ micro (10 megabecquerel millicurie meniscus The curved upper surface of a column of liquid. minute milliliter millimeter mass-to-charge ratio nano (10 negative polarity The inverse of a detector signal polarity. nanometer Nitrogen Phosphorous Detector On-Column Injector outside diameter ...
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Glossary Pulsed Discharge Detector Photoionization Detector Packed Column Injector part number PPKD Purged Packed Column Injector pounds per square inch Programmable Temperature Vaporizing Injector random access memory radio frequency read-only memory RS-232 industry standard for serial communications second S/SL Split/Splitless Injector surge slow average A gradual, long-term change in average RMS voltage level,...
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Thermal Conductivity Detector transient A brief voltage surge of up to several thousand volts, with a duration of less than 50 µs. Ultra Fast Module volt V ac volts, alternating current V dc volts, direct current Video Graphics Array Width Watt NOTE The symbol for a compound unit that is a quotient (for example, degrees Celsius per...
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Operating Sequences Replace the Septum ...........................30 Clean or Replace the Liner ........................34 Replace a Broken Liner ........................40 Replace the Split Line Tubing ......................48 Replace the Septum ...........................58 Clean or Replace the Liner ........................61 Replace a Broken Liner ........................67 Replace the Split Line Tubing ......................74 Replace the O-Ring ..........................83 Replace the Rotary Valve Seal ......................87 Replace the Rotary Valve Seal ......................101...
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Clean the Mirror Metal Plug ......................282 Clean the Flame-side Heat Shield ......................287 Replace the Jet ...........................292 Replace the Interferential Filter ......................297 Replace the Heat Shields ........................301 Replace the UV Lamp ........................319 Clean the Lamp Window ........................323 Checking for Leaks ..........................328 Clean or Replace the Collecting Electrode (FID on ECD) ..............349 Clean or Replace the Collecting Electrode (NPD on ECD) ..............356 Clean or Replace the Collecting Electrode (FPD on ECD) ...............363...