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Chapter 11

Maintaining a FID

FID Troubleshooting

214

Maintenance and Troubleshooting Manual

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.

Table 11-2.

Gases used for FID

Carrier gas

Detector Gas

Make-up gas Gas

Capillary Columns

Packed Columns

Helium
Nitrogen
Hydrogen

Helium
Nitrogen
Argon

Hy
Air

Nitrogen
(recommended)
Helium

The carrier gas flow range depends on the type of the gas used and on the type and
diameter of the capillary or packed column installed.

NOTE

Make-up gas is not required when a packed column is used.

The recommended range of detector gas flow rates tolerated by the FID are
reported in Table 11-3.

Table 11-3.

Recommended flow rates for FID

Gas

Flow rate

Hydrogen

30 - 50 mL/min

Air

300 - 600 mL/min

Make-up gas

10 - 60 mL/min

To gain optimum analytical performance from the FID the hydrogen flow rate
should be experimentally optimized, keeping the carrier and air flows constant, to
obtain the maximum signal intensity for the components of interest.

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Summary of Contents for TRACE GC Ultra

Page 1: ...Thermo Scientific TRACE GC Ultra Gas Chromatograph Maintenance and Troubleshooting Manual PN 31709180 Revision March 2011 Home ...

Page 2: ...rch 2011 Disclaimer Technical Information contained in this publication is for reference purposes only and is subject to change without notice Every effort has been made to supply complete and accurate information however Thermo Fisher Scientific assumes no responsibility and will not be liable for any errors omissions damage or loss that might result from any use of this manual or the information...

Page 3: ...y and performance only if installation re calibration changes and repairs have been carried out by authorized personnel and if the local installation complies with local law regulations the instrument is used according to the instructions provided and if its opera tion is only entrusted to qualified trained personnel Thermo Fisher Scientific is not liable for any damages derived from the non compl...

Page 4: ......

Page 5: ...the injector 29 When replacing the split line tubing 29 Chapter 3 Maintaining a Large Volume Splitless Injector 53 Large Volume Splitless Injector 54 Large Volume Splitless Injector Maintenance 56 When replacing the septum 56 When cleaning or replacing the liner 56 If the glass liner breaks inside the injector 57 When replacing the split line tubing 57 Chapter 4 Maintaining a Cold On Column Inject...

Page 6: ...he septum 124 Chapter 8 Maintaining a Purged Packed Column Injector 129 Purged Packed Column Injector 130 Purged Packed Column Injector Maintenance 132 When replacing the septum 132 When replacing the liner 132 Chapter 9 Maintaining a PTV Injector 141 PTV Injector 142 PTV Injector Maintenance 144 When replacing the septum 144 When cleaning or replacing the liner 145 If a liner breaks inside the in...

Page 7: ...n 217 Chapter 12 Maintaining an Electron Capture Detector 219 Electron Capture Detector ECD 220 ECD Maintenance 222 Wipe Test 223 Wipe Test Certificate 224 ECD Troubleshooting 235 Change in Sensitivity 235 Temperature 235 Gases 235 Contamination 236 Troubleshooting the ECD 237 Chapter 13 Maintaining a Nitrogen Phosphorus Detector 239 Nitrogen Phosphorus Detector NPD 240 NPD Maintenance 242 Thermio...

Page 8: ...nance 318 Leaks 318 PID Troubleshooting 334 Sensitivity 334 Lamp 334 Contamination 334 Troubleshooting the PID 335 Chapter 16 Maintaining a Thermal Conductivity Detector 337 Thermal Conductivity Detector TCD 338 TCD Maintenance 340 TCD Troubleshooting 341 Sensitivity 341 Baseline drift 341 Negative peaks 341 Troubleshooting the TCD 342 Chapter 17 Maintaining Detectors in Stack Configuration 345 EC...

Page 9: ... Regenerating Carrier and Split Lines Filters 387 Chapter 19 Analytical Troubleshooting 391 Appendix A Customer Communication 401 How To Contact Us 401 Reader Survey 402 Appendix B Reagents Safety Information 403 ACETONE 403 METHANOL 404 TOLUENE 404 Glossary 405 ...

Page 10: ...x Maintenance and Troubleshooting Manual Contents ...

Page 11: ...n and maintenance sequences for the Cold On Column injector for TriPlus autosampler Chapter 5 Maintaining a Cold On Column Injector Direct Narrow Bore reports information and maintenance sequences for the Cold On Column injector for direct injection into capillary column with the TriPlus autosampler Chapter 6 Maintaining a Cold On Column Injector reports information and maintenance sequences for t...

Page 12: ...tector Chapter 16 Maintaining a Thermal Conductivity Detector reports information and maintenance sequences for the Thermal Conductivity TCD detector Chapter 17 Maintaining Detectors in Stack Configuration reports information and maintenance sequences for detectors if installed in stack configuration Chapter 18 Analytical Troubleshooting is a guide to troubleshoot the instrument when its analytica...

Page 13: ...es messages or prompts displayed on the computer screen or on a digital display This symbol illustrates menu paths to select such as File Open KEY NAME Bold uppercase sans serif font indicates the name of a key on a keyboard or keypad such as ENTER CAUTION This symbol alerts you to an action or procedure that if performed improperly could damage the instrument NOTE This symbol alerts you to import...

Page 14: ... This symbol indicates the presence of flammable materials This symbol indicates the presence of radioactive material This symbol indicates an operation or procedure that must NOT be performed by the user A Thermo Fisher Scientific authorized Customer Support Engineer must perform this procedure This symbol indicates all metal objects such as watches and jewelry must be taken off This symbol indic...

Page 15: ...shooting Manual xv 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 ...

Page 16: ...ains 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 Both direct and alternating current 3 Three phase alternating current Earth ground terminal Protective conductor terminal Frame or chassis terminal Equipotentiality On Supply Off Supply ...

Page 17: ...ixture An explosion hazard could develop in the GC oven when hydrogen is used as a carrier gas if oven elements are not perfectly connected to each other or if the connection materials are worn out broken or otherwise faulty 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...

Page 18: ...installed contact your Thermo Fisher Scientific sales representative To comply with instrument safety requirements a Thermo Fisher Scientific CSE or authorized service technician should install the sensor If you plan to use a sensor other than the sensor recommended by Thermo Fisher Scientific you must verify its ability to perform the functions listed above before installing it It must comply wit...

Page 19: ... careful maintenance After the sensor is in use you must periodically check its operating performance and calibration as recommended by the manufacturer Refer to your hydrogen sensor s instruction manual for maintenance guidelines WARNING Never use hydrogen in your TRACE system unless your GC oven has a hydrogen sensor installed NOTE Thermo Fisher Scientific CSEs are not authorized to install or r...

Page 20: ......

Page 21: ...Maintenance and Troubleshooting Manual 21 1 Preventive Maintenance Chapter at a Glance Suggested Maintenance Schedule 22 ...

Page 22: ...ferent types will degrade at varying rates Factors affecting septa life include number of samples injected injector temperature condition of the syringe needle Our recommendations for septa replacement are based on 200 injections in a Thermo Fisher Scientific standard septum Septa from other manufacturers may show different rates of degradation Make sure you not only perform each scheduled item bu...

Page 23: ...pressure of gas cylinders Replace the cylinder when its pressure drops below 3500 kPa 35 bar or 500 psig Change S SL septum Change PTV septum Change PKD septum Change PPKD septum Change OC septum Perform the Leak Test procedure Monthly Check for leaks from the primary gas supply to the GC Semiannually Regenerate the S SL inlet vent line trap Regenerate the PTV inlet vent line trap Replace FID jet ...

Page 24: ...his operation 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 Clean or replace ECD source 1 As required by local law Perform wipe test on ECD1 Table 1 1 Standard Maintenance Schedule ...

Page 25: ...ining 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 ...

Page 26: ...Chapter 2 Maintaining a Split Splitless Injector Split Splitless Injector 26 Maintenance and Troubleshooting Manual Split Splitless Injector 6A 6B 6C 6D 6E 6F 6G 6H 18 ...

Page 27: ... 32 6D Liner splitless 5 mm ID 453 200 33 6E Liner for wide bore columns 453 003 10 6F Liner for polar solvents 453 003 20 6G Liner double gooseneck for nano volumes injection 45322080 6H Liner 0 8 mm ID 45352083 7 Liner seal 290 334 06 8 Injector body 9 Anti rotation plate 10 Washer 11 Retaining nut 12 Silver seal 290 336 29 13 Terminal fitting for capillary columns 347 054 51 14 Nut for terminal...

Page 28: ...for more information It is a good practice to change the septum with a new one every time the liner is replaced CAUTION The Injector temperature when high it makes a prematurely aging of the septum It is good practice to replace the septum of the S SL injector every week independently on the number of injections done When cleaning or replacing the liner The liner must be replaced periodically depe...

Page 29: ...453 200 32 Splitless injections 5 mm 453 200 33 Liner for direct injections into wide bore column 453 003 10 Laminar cup liner for split injections at high split flow rates or for the most polar solvents 453 003 20 If the glass 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...

Page 30: ... Therefore before beginning the sequence the injector must be cooled to room temperature PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 50 50 Initial time 2 Ramp 1 10 0 2 Scroll to Temp and press OFF 3 Press LEFT INLET or RIGHT INLET depending on which injector is operating In the following example a S SL injector installed on the right channel is c...

Page 31: ... When the inlet reaches the room temperature press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER S SL Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum holder with septum then the septum support ...

Page 32: ...ith your fingers 11 Clean the septum support from possible fragments left by the septum and reinsert it into the injector 12 Place the septum holder on the top of the septum support 13 Tighten the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance 14 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating...

Page 33: ...njector Maintenance and Troubleshooting Manual 33 16 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 17 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 ...

Page 34: ... 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 PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more information 1 While in s...

Page 35: ...led on the right channel is considered RIGHT INLET S SL Temp 250 250 Pressure 100 100 Mode split 4 Scroll to Temp and press OFF 5 When the inlet reaches the room temperature press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER S SL Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum ...

Page 36: ...CAUTION Be careful not to break the glass liner inside the injector when removing it Glass splinters might fall into the lower part of the vaporization chamber If the liner breaks refer to the Replace a Broken Liner Operating Sequence on page 40 11 If you are going to use a new liner go to step 14 If you are going to clean the liner put the dirty liner into an ultrasonic bath filled with a methano...

Page 37: ...e injector 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 14 Using tweezers insert the liner into the injector and push it gently towards the bottom fitting CAUTION Make sure you insert the bevelled end of the liner towards the bottom of the injector CAUTION Be care...

Page 38: ...nance and Troubleshooting Manual 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 ...

Page 39: ... the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance 21 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON 22 Press OVEN scroll to Temp and press ON 23 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 24 Perform a ...

Page 40: ...ure to avoid burns Therefore before beginning the sequence the injector must be cooled to room temperature PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 50 50 Initial time 2 Ramp 1 10 0 2 Scroll to Temp and press OFF 3 Press LEFT INLET or RIGHT INLET depending on which injector is operating In the following example a S SL injector installed on the ...

Page 41: ... 5 When the inlet reaches the room temperature press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER S SL Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum holder with septum then the septum support ...

Page 42: ...r Replace a Broken Liner 42 Maintenance and Troubleshooting Manual 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 ...

Page 43: ...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 15 With the aid of a pipe cleaner remove the possible glass fragments from the vaporization chamber ...

Page 44: ...nsert 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 position for instructions refer to the TRACE GC Operating Manual 19 Tighten the M4 retaining nut to hold the column in place ...

Page 45: ...m between the seal and the liner end 21 Using tweezers insert the liner into the injector and push it gently towards the bottom fitting Make sure you insert the bevelled end of the liner towards the bottom of the injector CAUTION Be careful not to damage the graphite seal or allow graphite to entering the liner Should this occur clean the liner with an inert gas 22 Tighten the liner cap using the ...

Page 46: ...m with your fingers 25 Clean the septum support from possible fragments left by the septum and reinsert it into the injector 26 Place the septum holder on the top of the septum support 27 Tighten the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance 28 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operat...

Page 47: ... Injector Maintenance and Troubleshooting Manual 47 30 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 31 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 ...

Page 48: ... at low temperature to avoid burns Therefore before beginning the sequence the injector must be cooled to room temperature PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 50 50 Initial time 2 Ramp 1 10 0 2 Scroll to Temp and press OFF 3 Press LEFT INLET or RIGHT INLET depending on which injector is operating In the following example a S SL injector i...

Page 49: ... which injector is operating RIGHT CARRIER S SL Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Remove the GC top cover a 1 Lift the detector cover off the GC top cover b 2 Open the oven door and unscrew the two top cover fastening screws c 3 Push the cover back about 1 cm and lift it up and off the GC 8 Split Line Tubing 1 8 Split Line Filter Split Line Connec...

Page 50: ...b 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 b Using two 8 10 mm wrenches unscrew and disconnect the split line tubing from the split line filter 10 Remove the split line tubing from the GC ...

Page 51: ...ding the fitting body steady tighten the nut tree quarters turn to the 9 o clock position 12 Connect the new split line tubing to the split line 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 b Insert the tubing into the outlet of the split line filter c Finger tighten the 6 MB nut until it start to grip the filter d...

Page 52: ...r is operating scroll to Temp and 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 leak detector to locate the possible leaks 17 When the injector is free of leaks reinstall the GC top cover 18 Set the normal injector and GC working condition ...

Page 53: ...rge 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 ...

Page 54: ...er 3 Maintaining a Large Volume Splitless Injector Large Volume Splitless Injector 54 Maintenance and Troubleshooting Manual 7 9 8 6 10 11 12 13 14 15 16 17 18 9 20 1 2 3 4 5 Large Volume Splitless Injector ...

Page 55: ...ional 2 453 220 67 10 Injector body 11 Anti rotation plate 12 Washer 13 Retaining nut 14 Silver seal 10 290 336 29 15 Terminal fitting for cap columns 347 054 51 16 Nut for terminal fitting 2 350 221 25 17 Graphite ferrule for 0 2 mm ID column 2 290 134 89 17 Graphite ferrule for 0 25 mm ID column 2 290 134 88 17 Graphite ferrule for 0 32 mm ID column 2 290 134 87 17 Graphite ferrule for 0 53 mm I...

Page 56: ...er to Chapter 19 Analytical Troubleshooting for more information It is a good practice to change the septum with a new one every time the liner is replaced 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 Typical symptoms will indicate that the liner must be replaced refer to...

Page 57: ...ks 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 Refer to Replace a Broken Liner Operating Sequence on page 67 for instructions When replacing the split line tubing Replace the sp...

Page 58: ...rns Therefore before beginning the sequence the injector must be cooled to room temperature PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 50 50 Initial time 2 Ramp 1 10 0 2 Scroll to Temp and press OFF 3 Press LEFT INLET or RIGHT INLET depending on which injector is operating In the following example a S SL injector installed on the right channel i...

Page 59: ... 5 When the inlet reaches the room temperature press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER S SL Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum from the septum holder use non metallic tools ...

Page 60: ... tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance 11 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON 12 Press OVEN scroll to Temp and press ON 13 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 14 Perform a leak check according to Per...

Page 61: ...harp 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 PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more information 1 While in stand by con...

Page 62: ...e right channel is considered RIGHT INLET S SL Temp 250 250 Pressure 100 100 Mode split 4 Scroll to Temp and press OFF 5 When the inlet reaches the room temperature press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER S SL Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Unscrew the ring nut and re...

Page 63: ...al CAUTION Be careful not to break the glass liner inside the injector when removing it Glass splinters might fall into the lower part of the vaporization chamber If the liner breaks refer to the Replace a Broken Liner Operating Sequence on page 67 11 If you are going to use a new liner go to step 14 If you are going to clean the liner put the dirty liner into an ultrasonic bath filled with a meth...

Page 64: ... 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 PRECAUTIONS 13 Using tweezers insert the liner into the injector and push it gently towards the bottom fitting CAUTION Make sure you insert the bevelled end of the liner towards the bottom of the injector ...

Page 65: ... 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 16 Tighten the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance ...

Page 66: ...R or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON 18 Press OVEN scroll to Temp and press ON 19 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 20 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 ...

Page 67: ...erature to avoid burns Therefore before beginning the sequence the injector must be cooled to room temperature PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 50 50 Initial time 2 Ramp 1 10 0 2 Scroll to Temp and press OFF 3 Press LEFT INLET or RIGHT INLET depending on which injector is operating In the following example a S SL injector installed on ...

Page 68: ...ss LEFT CARRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER S SL Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Unscrew the ring nut and remove the septum holder with the septum from the inlet port 9 Use the liner cap wrench provided with the GC to remove the injector liner cap ...

Page 69: ...litless Injector Maintenance and Troubleshooting Manual 69 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 Remove the analytical column with its ferrule ...

Page 70: ...e 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 With the aid of a pipe cleaner remove the possible glass fragments from the vaporization chamber 16 Reinsert the silver seal and the terminal fitting 17 Tighten the nut that retains the terminal fitting ...

Page 71: ...tructions refer to the TRACE GC Operating Manual 19 Tighten the M4 retaining nut to hold the column in place 20 Using tweezers insert the liner into the injector and push it gently towards the bottom fitting Make sure you insert the bevelled end of the liner towards the bottom of the injector CAUTION Be careful not to damage the graphite seal or allow graphite to entering the liner Should this occ...

Page 72: ...ded 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 23 Tighten the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance 24 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON ...

Page 73: ...nce and Troubleshooting Manual 73 25 Press OVEN scroll to Temp and press ON 26 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 27 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 ...

Page 74: ...ule M6x0 75 mm 6MB nut 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 PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 50 50 Initial time 2 Ramp 1 10 0 2 Scroll to Temp and press OFF 3 Press LEFT INLET or RIGHT INLET depending on which...

Page 75: ...RRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER S SL Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Remove the GC top cover a 1 Lift the detector cover off the GC top cover b 2 Open the oven door and unscrew the two top cover fastening screws c 3 Push the cover back about 1 cm and lift it up and off the GC 8 Look for the split lin...

Page 76: ...ng 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 b Using two 8 10 mm wrenches unscrew and disconnect the split line tubing from the split line filter 10 R e m o v e t h e s plit line tubing from the GC Split Line Tubing 1 8 Split Line Filter Split Line Connections ...

Page 77: ...ector 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 Fully insert the tubing into the fitting on the injector body and rotate the nut finger tight c Mark the nut at the 12 o clock position d While holding the fitting body steady tighten the nut tree quarters turn to the 9 o clock position ...

Page 78: ...o tighten the nut Use no more pressure than is necessary to obtain a good seal 13 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON 14 Press OVEN scroll to Temp and press ON 15 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 16 Perform a leak check according to Performing a Leak Check Ca...

Page 79: ...tions 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 83 Replace the Rotary Valve Seal 87 ...

Page 80: ...ng a Cold On Column Injector for Standard Automatic Injections Automated Operation Cold On Column Injector 80 Maintenance and Troubleshooting Manual Automated Operation Cold On Column Injector 1 2 7 8 9 B C D A 6 3 4 5 10 ...

Page 81: ...al Holder 350 014 71 5 O ring 290 013 02 6 OC base 299 022 56 7 Vespel ferrule for 0 25 mm ID column 290 134 61 7 Vespel ferrule for 0 32 mm ID column 290 134 60 7 Vespel ferrule for 0 53 mm ID column 290 134 71 8 Backwasher cooling sleeve for OC 452 000 01 9 Column retaining nut and backwasher for OC 452 100 01 10 Kit On Column Actuator for TriPlus Left The kit includes A Cold on column injector ...

Page 82: ... replaced at least every 200 injections or every time a problem related to O ring damage or wear occurs Refer to Chapter 19 Analytical Troubleshooting for more information The correct sequence is explained in the Operating Sequence Replace the O Ring on page 83 Possible leaks in the rotary valve Some symptoms particularly a low reproducibility in results may indicate that the connection between th...

Page 83: ... for TriPlus Sampler Materials needed Flat screwdriver O Ring See 5 Table 4 1 on page 81 Tweezers 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 70 70 Initial time 1 0 Ramp 1 20 0 2 Scroll to Temp and press OFF 3 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press OFF LEFT CARRIER OCI Pressure 30 0 30 0 Col ...

Page 84: ...ce the O Ring 84 Maintenance and Troubleshooting Manual 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 ...

Page 85: ...With the injection valve on the open position use an appropriate syringe needle 80 mm long to verify that the needle freely slides inside the injector WARNING Please verify that the syringe needle due to the friction exercised against the compressed O Ring seal enters with a reasonable applied force into the On Column injector port The needle must enter with some noticeable effort but smoothly and...

Page 86: ...6 Maintenance and Troubleshooting Manual 10 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON 11 Press OVEN scroll to Temp and press ON 12 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 ...

Page 87: ... 290 070 01 3 mm Allen wrench 4 mm Allen wrench 5 5 mm wrench 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 70 70 Initial time 1 0 Ramp 1 20 0 2 Scroll to Temp and press OFF 3 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press OFF LEFT CARRIER OCI Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 4 Remove th...

Page 88: ...ary Valve Seal 88 Maintenance and Troubleshooting Manual 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 ...

Page 89: ...oubleshooting Manual 89 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 9 A Loosen the two screws A on the side of the OC head Unscrew the remaining fixing screws of the head arm by using a 3 mm Allen wrench ...

Page 90: ... 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 The guide normally can be found inserted in the needle channel of the injector base or of the valve seal 11 Disassemble the injector body separating the head from the lower part ...

Page 91: ...y 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 assembly take care not to damage the inside of the head Eject the seal with the aid of a non metallic tool 15 Insert a new PTFE seal into its housing paying attention to the alignment of the holes 16 Insert the rotary valve into its housing 17 Fix the rotary valve w...

Page 92: ...Seal 92 Maintenance and Troubleshooting Manual 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 be allowed ...

Page 93: ...20 A 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 Reinstall the automatic actuator on the OC housing paying attention to insert the valve lever through the slot provided on the automatic actuator shaft Place the automatic actuator paying attention to not crush the cables under it ...

Page 94: ...ith the corresponding fixing holes located on the fixing arm of the OC head Fix the parts by using the two fixing screws 23 Reconnect the ground wire coming from the actuator motor 24 Reconnect the cables coming from the actuator and the TriPlus sampler to the control interface 25 Reposition the injector detector cover 26 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating...

Page 95: ...oll to Temp and press ON 29 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 30 Open Close 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 command OC Actuator The actuator move the OC valve lever as shown in the figure on the right ...

Page 96: ...Chapter 4 Maintaining a Cold On Column Injector for Standard Automatic Injections Replace the Rotary Valve Seal 96 Maintenance and Troubleshooting Manual ...

Page 97: ... 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 ...

Page 98: ...ter 5 Maintaining a Cold On Column Injector Direct Narrow Bore Automated Operation Cold On Column Injector 98 Maintenance and Troubleshooting Manual Automated Operation Cold On Column Injector 1 2 6 7 3 4 5 ...

Page 99: ... P N 1 Seal PTFE 290 071 06 2 Clip 426 003 57 3 Needle guide set of 2 453 220 63 4 OC base 299 022 56 5 Vespel ferrule for 0 25 mm ID column 290 134 61 5 Vespel ferrule for 0 32 mm ID column 290 134 60 5 Vespel ferrule for 0 53 mm ID column 290 134 71 6 Backwasher cooling sleeve for OC 452 000 01 7 Column retaining nut and backwasher for OC 452 100 01 On Column injector head assy 299 022 48 Kit up...

Page 100: ...er Possible leaks in the rotary valve Some symptoms particularly a low reproducibility in results may indicate that the connection between the rotary valve and the relevant PTFE seal is not in good condition Refer to Chapter 19 Analytical Troubleshooting for more information To eliminate possible leaks on the rotary valve tighten the Allen screws that fix the upper and the lower parts of the injec...

Page 101: ...106 3 mm Allen wrench 4 mm Allen wrench 5 5 mm wrench 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 70 70 Initial time 1 0 Ramp 1 20 0 2 Scroll to Temp and press OFF 3 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press OFF LEFT CARRIER OCI Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 4 Remove the inject...

Page 102: ...e Seal 102 Maintenance and Troubleshooting Manual 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 ...

Page 103: ...oting Manual 103 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 9 A Loosen the two screws A on the side of the OC head Unscrew the remaining fixing screws of the head arm by using a 3 mm Allen wrench ...

Page 104: ...len 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 The guide normally can be found inserted in the needle channel of the injector base or of the valve seal 11 Disassemble the injector body separating the head from the lower part ...

Page 105: ... 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 assembly take care not to damage the inside of the head Eject the seal with the aid of a non metallic tool 15 Insert a new PTFE seal into its housing paying attention to the alignment of the holes 16 Insert the rotary valve into its housing 17 Fix the rotary valve with the...

Page 106: ... Maintenance and Troubleshooting Manual 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 be allowed ...

Page 107: ...x 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 Reinstall the automatic actuator on the OC housing paying attention to insert the valve lever through the slot provided on the automatic actuator shaft Place the automatic actuator paying attention to not crush the cables under it ...

Page 108: ... corresponding fixing holes located on the fixing arm of the OC head Fix the parts by using the two fixing screws 23 Reconnect the ground wire coming from the actuator motor 24 Reconnect the cables coming from the actuator and the TriPlus sampler to the control interface 25 Reposition the injector detector cover 26 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll...

Page 109: ...Temp and press ON 29 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 30 Open Close 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 command OC Actuator The actuator move the OC valve lever as shown in the figure on the right ...

Page 110: ...Chapter 5 Maintaining a Cold On Column Injector Direct Narrow Bore Replace the Rotary Valve Seal 110 Maintenance and Troubleshooting Manual ...

Page 111: ...l 111 6 Maintaining a Cold On Column Injector Chapter at a Glance Manual Cold On Column Injector 112 Cold On Column Injector Maintenance 114 Cold On Column Injector Maintenance 114 Operating Sequences Replace the Rotary Valve Seal 115 120 ...

Page 112: ...Chapter 6 Maintaining a Cold On Column Injector Manual Cold On Column Injector 112 Maintenance and Troubleshooting Manual Manual Cold On Column Injector ...

Page 113: ...valve 290 070 01 8 Rotary valve retaining clip 426 003 57 9 Needle guide 453 220 36 10 Vespel ferrule for 0 25 mm ID column 290 134 61 Vespel ferrule for 0 32 mm ID column 290 134 60 Vespel ferrule for 0 53 mm ID column 290 134 71 11 Backwasher cooling sleeve 452 000 01 12 Column retaining nut and backwasher 452 100 01 Chapter 6 Manual Cold On Column Injector Maintaining a Cold On Column Injector ...

Page 114: ...replaced by the user Possible leaks in the rotary valve Some symptoms particularly a low reproducibility in results may indicate that the connection between the rotary valve and the relevant PTFE seal is not in good condition Refer to Chapter 19 Analytical Troubleshooting for more information To eliminate possible leaks on the rotary valve tighten the Allen screws that fix the upper and the lower ...

Page 115: ... needed 5 5 mm hexagonal wrench PTFE seal P N 290 070 01 3 mm Allen wrench 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 70 70 Initial time 1 0 Ramp 1 20 0 2 Scroll to Temp and press OFF 3 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press OFF LEFT CARRIER OCI Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 ...

Page 116: ...ctuation 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 CAUTION Pay attention not to lose the small needle guide when removing the injector body The guide normally can be found inserted in the needle channel of the injector base or of the valve seal ...

Page 117: ...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 11 Push the PTFE seal upwards to eject it CAUTION In order to avoid leaks of sample from the valve assembly take care not to damage the inside of the head Eject the seal with the aid of a non metallic tool ...

Page 118: ...eal 118 Maintenance and Troubleshooting Manual 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 Reassemble the two parts of the injector body ...

Page 119: ... 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 be allowed 18 Reposition the injector detector cover 19 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON ...

Page 120: ...umn Injector Replace the Rotary Valve Seal 120 Maintenance and Troubleshooting Manual 20 Press OVEN scroll to Temp and press ON 21 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 ...

Page 121: ...enance and Troubleshooting Manual 121 7 Maintaining a Packed Column Injector Chapter at a Glance Packed Column Injector 122 Packed Column Injector Maintenance 124 Operating Sequences Replacing the Septum 125 ...

Page 122: ...Chapter 7 Maintaining a Packed Column Injector Packed Column Injector 122 Maintenance and Troubleshooting Manual Packed Column Injector ...

Page 123: ...Retaining nut 6 Spacer 453 020 48 7 Septum 313 032 00 High Temperature septum 313 032 09 8 Adapter 9 Retaining nut for adapter 350 401 18 10 Brass ferrule for adapter 290 341 37 11 Retaining nut and ferrule for adapter 350 201 17 Chapter 7 Packed Column Injector Maintaining a Packed Column Injector Maintenance and Troubleshooting Manual 123 ...

Page 124: ...sher Scientific authorized technical personnel In order to keep the injector operating at peak performance you should periodically replace the septum When replacing the septum The septum must be replaced at least every 200 injections or every time a problem occurs related to a septum damage or wear Refer to Chapter 19 Analytical Troubleshooting for more information Instructions are reported in the...

Page 125: ...to avoid burns Therefore before beginning the sequence the injector must be cooled to room temperature PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 80 80 Initial time 20 Ramp 1 Off 2 Scroll to Temp and press OFF 3 Press LEFT INLET or RIGHT INLET depending on which injector is operating In the following example a PKD injector installed on the right...

Page 126: ...nual 5 When the inlet reaches the room temperature press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER PKD Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum using a non metallic sharp tool ...

Page 127: ... Do not overtighten the injector cap You could damage the septum and affect performance 11 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON 12 Press OVEN scroll to Temp and press ON 13 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 14 Perform a leak check according to Performing a Leak...

Page 128: ......

Page 129: ...g Manual 129 8 Maintaining a Purged Packed Column Injector Chapter at a Glance Purged Packed Column Injector 130 Purged Packed Column Injector Maintenance 132 Operating Sequences Replace the Septum 133 Clean or Replace the Liner 136 ...

Page 130: ...Chapter 8 Maintaining a Purged Packed Column Injector Purged Packed Column Injector 130 Maintenance and Troubleshooting Manual Purged Packed Column Injector 11 12 1 7 6 13 2 3 4 5 8 8A 8B 10 9 ...

Page 131: ...igh Temperature septum 313 032 09 8A Liner wide bore 2 mm 453 220 49 8B Liner wide bore 4 mm 453 220 50 9 Adapter for wide bore columns 347 003 03 10 Retaining nut 350 024 04 11 Graphite ferrule for 0 53 mm ID column 290 134 85 12 Fixing nut for column 350 324 23 13 Liner seal 290 334 05 Chapter 8 Purged Packed Column Injector Maintaining a Purged Packed Column Injector Maintenance and Troubleshoo...

Page 132: ...ry 200 injections or every time a problem occurs related to a septum damage or wear Refer to Chapter 19 Analytical Troubleshooting for more information Instructions are reported in the Replace the Septum Operating Sequence on page 133 It is good practice to replace the septum every time the liner is replaced When replacing the liner The liner must be replaced periodically depending on the number o...

Page 133: ...id burns Therefore before beginning the sequence the injector must be cooled to room temperature PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 80 80 Initial time 200 Ramp 1 Off 2 Scroll to Temp and press OFF 3 Press LEFT INLET or RIGHT INLET depending on which injector is operating In the following example a PPKD injector installed on the right cha...

Page 134: ...Manual 5 When the inlet reaches the room temperature press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER PPKD Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum using a non metallic sharp tool ...

Page 135: ...ON Do not overtighten the injector cap You could damage the septum and affect performance 11 Press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON 12 Press OVEN scroll to Temp and press ON 13 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 14 Perform a leak check according to Performing a Le...

Page 136: ...ING 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 PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more information 1 While in stand by condition press OVEN to access the oven control ...

Page 137: ...d on the right channel is considered RIGHT INLET PPKD Temp 200 200 Pressure 30 30 Mode Wide Bore 4 Scroll to Temp and press OFF 5 When the inlet reaches the room temperature press LEFT CARRIER or RIGHT CARRIER depending on which injector is operating RIGHT CARRIER PPKD Col flow 3 0 Pressure 30 30 Flow mode con pres 6 Scroll to Pressure and press OFF 7 Unscrew the nut that retains the analytical co...

Page 138: ...jector 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 an hour 13 Using tweezers remove the liner from the bath and dry it with compressed clean air PRECAUTIONS ...

Page 139: ...e injector and push it gently upwards 16 Tighten the retaining nut to close the bottom of the injector NOTE For trace analysis you should pre treat the liner with a suitable silylating reagent prior to inserting it into the injector 17 Insert the analytical column with its ferrule into the bottom of the injector in its previous position For detailed instructions refer to the TRACETM GC Ultra Opera...

Page 140: ...ntenance and Troubleshooting Manual 20 Press OVEN scroll to Temp and press ON 21 Press LEFT INLET or RIGHT INLET depending on which injector is operating scroll to Temp and press ON 22 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 ...

Page 141: ...intaining 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 ...

Page 142: ...Chapter 9 Maintaining a PTV Injector PTV Injector 142 Maintenance and Troubleshooting Manual PTV Injector 14 12 15 16 5a 4a Column Side Injection Side 14a A B C D E F G H I L M 7 ...

Page 143: ...34 20 7A Silcosteel liner 2 mm ID 453 220 44 7B Silcosteel liner 1 mm ID 453 220 46 7C Glass liner 2 mm ID 453 220 45 7D Deactivated glass liner 1 mm ID 453 220 54 7E Silcosteel liner for simile On column injections 453 220 52 7F Silcosteel liner for Large Volume Injections 453 220 56 7G Glass sintered deactivated liner for Large Volume Injections 453 220 60 7H Deactivated glass liner with baffles...

Page 144: ... N 365 020 01 the septum of your PTV injector should be replaced after about 200 injections The septum should be also replaced every time a problem that is related to septum damage or wear occurs refer to Chapter 19 Analytical Troubleshooting for more information 10 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 co...

Page 145: ...h a new one or clean the liner and reinstall it Table 9 2 shows the available types of liners for the PTV injector Table 9 2 Available liners for PTV injector Application P N Silcosteel liner 2 mm ID provided with the GC 453 220 44 Silcosteel liner 1 mm ID provided with the GC 453 220 46 Glass liner 2 mm ID 453 220 45 Glass liner 1 mm ID 453 220 54 Silcosteel liner for simile On column injections ...

Page 146: ... 157 Adjusting the quartz wool packing PTV injector arranged for Large Volume injections can be fitted with a liner see Available liners for PTV injector page 145 6 packed with quartz wool A casual increase of pressure inside the liner or removing the column without closing the carrier gas pressure could cause the packing glide towards the bottom of the liner altering the conditions of sample reco...

Page 147: ...is operation must be carried out at low temperature to avoid burns Therefore before beginning the sequence the injector must be cooled to room temperature PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 50 50 Initial time 1 Ramp 1 10 0 2 Scroll to Temp and press OFF 3 Press RIGHT INLET RIGHT INLET PTV Temp 50 50 Pressure 100 100 Mode split 4 Scroll t...

Page 148: ...roubleshooting Manual 5 When the inlet reaches the room temperature press RIGHT CARRIER RIGHT CARRIER PTV Pressure 30 0 30 0 Col flow 3 00 Lin Veloc 60 9 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum holder with septum then the septum support ...

Page 149: ...d touching the septum with your fingers 11 Clean the septum support from possible fragments left by the septum and reinsert it into the injector 12 Place the septum holder on the top of the septum support 13 Tighten the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance 14 Press RIGHT CARRIER scroll to Pressure and press ON 1...

Page 150: ... Injector Replace the Septum 150 Maintenance and Troubleshooting Manual 16 Press RIGHT INLET scroll to Temp and press ON 17 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 ...

Page 151: ...p 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 PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more information 1 While in stand by condit...

Page 152: ...ressure 100 100 Mode split 4 Scroll to Temp and press OFF 5 When the inlet reaches the room temperature press RIGHT CARRIER depending on which injector is operating RIGHT CARRIER PTV Col flow 2 5 Pressure 100 100 Flow mode con pres 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum holder with septum then the septum support ...

Page 153: ... glass liner be careful not to break it inside the injector when removing it Glass splinters might fall into the lower part of the vaporization chamber If the liner breaks refer to the Replace a Broken Liner Operating Sequence on page 157 11 If you are going to replace the liner with a new one go to step 13 If you are going to clean the liner put the dirty liner into an ultrasonic bath filled with...

Page 154: ... 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 14 Using tweezers insert the liner into the injector and push it gently towards the bottom fitting CAUTION Be careful not to damage the graphite seal or allow graphite to entering the liner Should this occur clean the liner with an i...

Page 155: ...roubleshooting Manual 155 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 ...

Page 156: ...h the septum 20 Tighten the injector cap to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance 21 Press RIGHT CARRIER scroll to Pressure and press ON 22 Press OVEN scroll to Temp and press ON 23 Press RIGHT INLET scroll to Temp and press ON 24 Perform a leak check according to Performing a Leak Check Capillary Column Operating Sequence on pa...

Page 157: ...e 9 2 on page 145 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 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 50 50 Initial time 1 Ramp 1 10 0 2 Scroll to Temp and press OFF 3 Press RIGHT INLET RIGHT INLET PTV Temp 50 50 Pressure 100 ...

Page 158: ... Troubleshooting Manual 5 When the inlet reaches the room temperature press RIGHT CARRIER RIGHT CARRIER PTV Col flow 2 5 Pressure 100 100 Flow mode con pres 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum holder with septum then the septum support ...

Page 159: ...ining a PTV Injector Maintenance and Troubleshooting Manual 159 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 ...

Page 160: ...mn 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 CAUTION The spacer placed below the liner will also be ejected from the injector pay attention not to lose it ...

Page 161: ...ation 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 16 Using tweezers insert the liner into the injector and push it gently towards the bottom CAUTION Be careful not to damage the graphite seal or allow graphite to entering the liner Should this occur clean the liner with an inert gas PRECAUTIONS ...

Page 162: ...to the bottom of the injector in its previous position Refer to the TRACE GC Operating Manual for instructions NOTE In split and splitless injection modes the distance d between the top of the capillary column and the ferrule must be 3 cm If you are using a simile on column liner in order to operate in on column injection mode insert the column as far as it goes 19 Tighten the M4 retaining nut to ...

Page 163: ...3 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 Place the septum support into its housing inside the injector 23 Reinsert the septum holder with the septum ...

Page 164: ...N Do not overtighten the injector cap You could damage the septum and affect performance 25 Press RIGHT CARRIER scroll to Pressure and press ON 26 Press OVEN scroll to Temp and press ON 27 Press RIGHT INLET scroll to Temp and press ON 28 Perform an automatic leak check according to Performing a Leak Check Capillary Column Operating Sequence on page 181 ...

Page 165: ... bar e g 1 6 mm PEEK tube 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 PRECAUTIONS 1 While in stand by condition press OVEN to access the oven control table OVEN Temp 50 50 Initial time 5 Ramp 1 10 0 2 Scroll to Temp and press OFF 3 Press RIGHT INLE...

Page 166: ...and Troubleshooting Manual 5 When the inlet reaches the room temperature press RIGHT CARRIER RIGHT CARRIER PTV Col flow 2 5 Pressure 100 100 Flow mode con pres 6 Scroll to Pressure and press OFF 7 Unscrew the injector cap 8 Remove the septum holder with septum then the septum support ...

Page 167: ...ded 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 CAUTION Be careful not to damage the graphite seal or allow graphite to entering the liner Should this occur clean the liner with an inert gas PRECAUTIONS ...

Page 168: ...e liner CAUTION Do not compress the wool to avoid carrier gas cannot flow through the liner 13 Place a new graphite seal over the liner making sure to leave a distance of about 10 mm between the seal and the liner end 14 Using tweezers insert the liner into the injector and push it gently towards the bottom fitting CAUTION Be careful not to damage the graphite seal or allow graphite to entering th...

Page 169: ...Troubleshooting Manual 169 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 ...

Page 170: ... to finger tight CAUTION Do not overtighten the injector cap You could damage the septum and affect performance 21 Press RIGHT CARRIER depending on which injector is operating scroll to Pressure and press ON 22 Press OVEN scroll to Temp and press ON 23 Press RIGHT INLET depending on which injector is operating scroll to Temp and press ON 24 Perform a leak check according to Performing a Leak Check...

Page 171: ...he sample may be caused by operating conditions set incorrectly with regard to the chosen injection mode Discrimination could also be caused by degradation of the thermally labile compounds due to the cathalytic effect of bad deactivated quartz wool inside the liner by products originated in previous injections that have been not completely eliminated from the liner during the cleaning phase or th...

Page 172: ...temp to a value closer to the solvent boiling point Flooding of the liner due to low injection temperature Set Inject temp to a higher value If the symptom does not disappear insert quartz wool in the liner Refer to Adjust a Quartz Wool Packing Operating Sequence on page 165 Flooding of the liner due to injected volume too large Reduce the amount of sample to be injected Replace the liner with one...

Page 173: ...volatile compounds in splitless mode Initial temperature too high Set Inject temp to a lower value Liner diameter too small Replace the liner with one of larger diameter Refer to Clean or Replace the Liner Operating Sequence on page 151 Volatiles are eliminated through the purge line Set Const purge flow to N then set Stop purge for to a value corresponding to Splitless time Discrimination of vola...

Page 174: ...eplace the Liner Operating Sequence on page 151 Lack of an adequate quartz wool packing inside the liner Replace the packed liner with a new one filled will quartz wool Fix the quartz wool packing inside the liner Refer to Adjust a Quartz Wool Packing Operating Sequence on page 165 Excessive broadening of the solvent peak Volatile compounds obscured Lack of sensitivity Injection pressure set too h...

Page 175: ...aller diameter to improve transfer efficiency Refer to Clean or Replace the Liner Operating Sequence on page 151 Cathalytic and thermal degradation of sensitive compounds caused by the quartz wool inside the liner Use a new packed liner If the symptom does not disappear use an empty liner Refer to Clean or Replace the Liner Operating Sequence on page 151 Table 9 3 PTV Troubleshooting Table Continu...

Page 176: ...ower value Lack of an adequate quartz wool packing inside the liner Fix the quartz wool packing inside the liner Refer to Adjust a Quartz Wool Packing Operating Sequence on page 165 Replace the liner with another filled with quartz wool Refer to Clean or Replace the Liner Operating Sequence on page 151 Discrimination of volatile compounds Injection speed set too low Set Inject speed to a higher va...

Page 177: ...n of sensitive compounds caused by products accumulated on the quartz wool Replace the packed liner with a new one Refer to Clean or Replace the Liner Operating Sequence on page 151 Table 9 5 PTV General Troubleshooting Symptom Diagnosis Remedy Broadening or loss of peaks at the end of the chromatogram Injector temperature too low Increase the injector temperature Premature cooling of the injector...

Page 178: ...Chapter 9 Maintaining a PTV Injector PTV Troubleshooting 178 Maintenance and Troubleshooting Manual ...

Page 179: ...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 ...

Page 180: ...ector base body Check the accessible critical connections column to injector column to detector split and purge valves septum caps A possible leak source may be the gas bottles gas chromatograph connections Check these lines before the others if specific symptoms indicate that the leak is outside the gas chromatograph DCC equipped systems TRACE GC Ultra equipped with a DCC Digital Carrier Control ...

Page 181: ... shown in Figure 10 1 Flowmeter connection fitting Knurled nuts Blind channel for leak check Open channel for 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 perform...

Page 182: ... on the configuration of your GC In the example the left column is considered LEAK CHECK COLUMN Right column1 Left column1 1 This item appears if the relevant channel is present and configured 4 Scroll to the channel of interest and press ENTER to open the following menu L COL LEAK CHECK Start Leak Check Leak Check Settings 5 Scroll to Leak Check Settings and press ENTER to open the relevant menu ...

Page 183: ... leak check command to start the operation The split and purge valves of the selected channel are automatically closed and the channel is pressurized with carrier gas to the leak check set point CHECKING L COLUMN Pressure 200 Elapsed time 0 90 Use STOP to abort NOTE To abort Leak Check press STOP A relevant message will be displayed 10 The system is pressurized for one minute then the pressure val...

Page 184: ...aks 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 If the leaks cannot be located contact your customer support organization Refer to Appendix B Customer Communication for contact information ...

Page 185: ... 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 3 Only for FPD remove the jet In case of capillary columns use typewriter correction fluid to mark the position of the column entering the detector base body Lower the column end down to the top of the detector base body then tighten the M4 fixing n...

Page 186: ...pressure pressurization value at which the leak check must be performed The range is comprised from 10 to 999 kPa 1 45 145 psi 11 In Sensitivity line set the maximum value the pressure can drop during the test The range is comprised from 1 to 10 kPa 0 145 1 45 psi 12 Press CLEAR to exit Leak Check Settings menu and return to the previous menu L COL LEAK CHECK Start leak check Leak Check settings 1...

Page 187: ...f the pressure does not drop more than the Sensitivity set value the message Leak check passed is displayed R L LEAK CHECK COMPLETED SUCCESSFULLY Leak check passed If not the message Leak detected is displayed indicating possible leaks in the system 15 If leaks are detected check the accessible critical connections with an electronic leak detector to locate the possible leaks 16 Eliminate the leak...

Page 188: ...leak detector or equivalent handheld electronic leak detector to find possible leaks Multiple systems If more than a system is attached to the same gas source you will need to isolate each GC system 1 Install a cut off valve and pressure gauge with an 1 8 inch input tee in the gas line leading to the GC that you are leak testing as shown in Figure 10 3 Be sure the pressure gauge is connected in li...

Page 189: ...alve Pressure Gauge 1 8 Tee with Teflon Tape to Seal Pipe Threads Chapter 10 Leak Test the Lines from the Gas Source to the GC Ensuring Tightness Maintenance and Troubleshooting Manual 189 Figure 10 3 Testing Multiple Systems ...

Page 190: ...Chapter 10 Ensuring Tightness Leak Test the Lines from the Gas Source to the GC 190 Maintenance and Troubleshooting Manual ...

Page 191: ...D 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 ...

Page 192: ...Chapter 11 Maintaining a FID Flame Ionization Detector FID 192 Maintenance and Troubleshooting Manual Flame Ionization Detector FID 12 ...

Page 193: ...de 259 011 15 5 Retaining screw 311 060 08 6 Jet 404 043 01 7 Collecting electrode pin 206 016 02 8 Flame ignition coil polarization assembly 206 016 03 9 Ceramic insulator 302 023 10 10 Jet removing tool 205 019 00 11 Detector base body 12 Spring contact 206 031 00 Chapter 11 Flame Ionization Detector FID Maintaining a FID Maintenance and Troubleshooting Manual 193 ...

Page 194: ... 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 cleaning the jet replacing the jet cleaning the collecting electrode replacing the collecting electrode replacing the ignition assembly ...

Page 195: ...s Distiller water Clean compressed air GC grade methanol Clean paper towel 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 PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more i...

Page 196: ...LEFT DETECTOR or RIGHT DETECTOR depending on the location of the FID detector to access the FID control table In the following example a FID installed on the right channel is considered 2 Scroll to Flame and press OFF 3 Scroll subsequently to Base temp H2 and Air and press OFF 4 Disconnect the signal and ignition polarization cables from the detector 5 Loosen the fixing screw on the front of the d...

Page 197: ...al 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 9 Place the jet on a paper towel and let it air dry PRECAUTIONS 10 When the jet is dry place the jet into the housing and tighten it with the proper tool Ensure the jet is perfectly vertically aligned to avoid damaging its ceramic part v ...

Page 198: ...1 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 Refer to the relevant chapter of the TRACE GC Ultra Operating manual for more information ...

Page 199: ...s Therefore before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS 1 RIGHT DETECTOR FID Flame Off Base temp 300 300 Signal pA 5 4 Ign tresh 2 0 Flameout retry Off H2 35 Off Air 350 Off Mkup N2 30 30 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the FID detector to access the FID control table In the following example a FID installed on the ri...

Page 200: ...tenance and Troubleshooting Manual 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 ...

Page 201: ...ctly 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 9 Reconnect the signal and ignition cables to the detector 10 Reset the detector to the required operating conditions Refer to the relevant chapter of the TRACETM GC Ultra Operating manual for more information ...

Page 202: ...leaning 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 Therefore before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Informatio...

Page 203: ...CTOR or RIGHT DETECTOR depending on the location of the FID detector to access the FID control table In the following example a FID installed on the right channel is considered 2 Scroll to Flame and press OFF 3 Scroll subsequently to Base temp H2 and Air and press OFF 4 Disconnect the signal and ignition cables from the detector 5 Loosen the fixing nut on the front of the detector cell and remove ...

Page 204: ...screw and remove the gold contact pin 9 Using tweezers extract the collecting electrode through the top of the detector cell 10 Place the collecting electrode in the ultrasonic bath filled with liquid detergent and clean it for about five minutes 11 Handle the collecting electrode with forceps or tweezers rinse it using distilled water then methanol 12 Place the collecting electrode on a paper tow...

Page 205: ...oubleshooting Manual 205 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 Remount the connector holder assembly verifying the contact efficiency ...

Page 206: ...e 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 19 Reset the detector to the required operating conditions Refer to the relevant chapter of the TRACETM GC Ultra Operating manual for more information ...

Page 207: ...burns Therefore before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS 1 RIGHT DETECTOR FID Flame Off Base temp 300 300 Signal pA 5 4 Ign tresh 2 0 Flameout retry Off H2 35 Off Air 350 Off Mkup N2 30 30 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the FID detector to access the FID control table In the following example a FID installed on th...

Page 208: ... 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 7 Remove the holder assembly of the signal cable by unscrewing the two fixing screws 8 Using forceps unscrew and remove the gold contact pin 9 Using tweezers extract the collecting electrode through the top of the detector cell ...

Page 209: ...oubleshooting Manual 209 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 Remount the connector holder assembly verifying the contact efficiency ...

Page 210: ...he 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 16 Reset the detector to the required operating conditions Refer to the relevant chapter of the TRACETM GC Ultra Operating manual for more information ...

Page 211: ...e before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS 1 RIGHT DETECTOR FID Flame Off Base temp 300 300 Signal pA 5 4 Ign tresh 2 0 Flameout retry Off H2 35 Off Air 350 Off Mkup N2 30 30 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the FID detector to access the FID control table In the following example a FID installed on the right channe...

Page 212: ...enance and Troubleshooting Manual 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 ...

Page 213: ...g fork is placed downwards to achieve the correct contact with the jet 8 Place the detector cell on the detector base body and tighten the retaining screw 9 Reconnect the signal and ignition cables to the detector 10 Reconnect the signal and ignition cables to the detector 11 Reset the detector to the required operating conditions Refer to the relevant chapter of the TRACETM GC Ultra Operating man...

Page 214: ...ogen Hydrogen Helium Nitrogen Argon Hydrogen Air Nitrogen recommended Helium The carrier gas flow range depends on the type of the gas used and on the type and diameter of the capillary or packed column installed NOTE Make up gas is not required when a packed column is used The recommended range of detector gas flow rates tolerated by the FID are reported in Table 11 3 Table 11 3 Recommended flow ...

Page 215: ... min 40 mL min Hydrogen 35 mL min 40 mL min Air 350 mL min 500 mL min Make up gas Nitrogen 30 mL min Not used For high sensitivity applications it is essential that you exclude all traces of organic contamination from the chromatographic system and or from the gas lines of the detector Such contamination would cause ghost peaks in the chromatogram or more commonly an unstable baseline WARNING It i...

Page 216: ... Remedy Incorrect fuel gas flows Make sure that all flows are correct Defective igniter Check the igniter element Refer to the Replace the Ignition Assembly Operating Sequence on page 211 for instructions Broken or cracked flame jet Replace jet Refer to the Replace the Jet Operating Sequence on page 199 for instructions Blocked jet tip Check for a blocked jet by measuring the hydrogen flow with th...

Page 217: ...n 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 ...

Page 218: ......

Page 219: ...an Electron Capture Detector Chapter at a Glance Electron Capture Detector ECD 220 ECD Maintenance 222 Wipe Test 223 ECD Troubleshooting 235 Operating Sequences Clean the Collecting Electrode 226 Replace the Collecting Electrode 229 Replace the Silver Seal 232 ...

Page 220: ...Chapter 12 Maintaining an Electron Capture Detector Electron Capture Detector ECD 220 Maintenance and Troubleshooting Manual Electron Capture Detector ECD ...

Page 221: ...ctor 5 Signal connector 6 Detector cover 7 Collecting electrode 277 003 50 8 Silver seal 290 150 58 9 Temperature sensor heater assembly 190 500 87 10 ECD fixing tool 205 021 50 11 Seal 290 326 08 Maintenance kit 19050221 Chapter 12 Electron Capture Detector ECD Maintaining an Electron Capture Detector Maintenance and Troubleshooting Manual 221 ...

Page 222: ...tact your local Thermo Fisher Scientific Technical Service office for maintenance or replacement of the source whichever is necessary Strictly follow the existing regulations for the transport of radioactive material WARNING The Electron Capture Detector ECD contains a 63 Ni beta emitting radioactive source of 370 MBq 10 mCi The 63 Ni radioisotope electrically deposited as metal on a nickel foil i...

Page 223: ...he Wipe Test method Each detector is provided with a Wipe Test Certificate reporting the results of the values found and the procedure followed NOTE The users of the ECD detector in the United States are required to perform a Wipe Test on their ECD at intervals not exceeding 3 years 36 months following the reported procedure For other Countries please refer to the appropriate agency for equivalent...

Page 224: ... Detector Model Detector Serial Number ASSAY RESULTS Observed Counting Rate Radionuclide Counting Efficiency Background c p m c p m net d p m Activity Bq 63 Ni Method described overleaf Sum of measurement taken ASSAY OF RESULTS The radioactive integrity of the detector is within the stated limits The detectable activity is less than 185 Bq Wipe Test performed by Date Analysis performed by Date ...

Page 225: ...new cotton wool swabs and place in clean marked vial Submit the marked vials containing the swabs for the radioactivity measurement using a liquid scintillation counter Notes The wipe test should be performed on the ECD at room temperature Radioactivity should be measured by a liquid scintillation spectrometer TRI CARB Packard or similar discriminating at 1 70 keV to encompass the maximum beta ene...

Page 226: ...erations involving the radioactive source must be performed ONLY by qualified personnel duly authorized to handle radioactive material Please contact your local Thermo Fisher Scientific Technical Service office WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more information WARNING This operation must be...

Page 227: ...rent nA 1 0 Freq kHz 2 15 Pulse amp V 25 Pulse width us 1 0 Mkup N2 40 Off 2 Scroll subsequently to Base temp and ECD temp and press OFF 3 Scroll to Mkup N2 and press OFF 4 Disconnect the signal excitation and heater cables from the detector 5 Remove the cover and the detector chimney unscrewing the two retaining Allen screws Use a 1 5 mm Allen wrench 6 Unscrew the collecting electrode and remove ...

Page 228: ...Electrode 228 Maintenance and Troubleshooting Manual 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 ...

Page 229: ...g the radioactive source must be performed ONLY by qualified personnel duly authorized to handle radioactive material Please contact your local Thermo Fisher Scientific Technical Service office WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more information WARNING This operation must be carried out at l...

Page 230: ...nnel is considered RIGHT DETECTOR ECD Base temp 250 Off ECD temp 250 Off Ref current nA 1 0 Freq kHz 2 15 Pulse amp V 25 Pulse width us 1 0 Mkup N2 40 Off 2 Scroll subsequently to Base temp and ECD temp and press OFF 3 Scroll to Mkup N2 and press OFF 4 Disconnect the signal excitation and heater cables from the detector 5 Remove the cover and the detector chimney unscrewing the two retaining Allen...

Page 231: ...ntenance and Troubleshooting Manual 231 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 10 Reset the detector to the required operating conditions ...

Page 232: ...Thermo Fisher Scientific Technical Service office 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 PRECAUTIONS 1 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the ECD to access the ECD control table In the following example an ECD installed on the right channel i...

Page 233: ...nual 233 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 6 Remove the detector from its base body 7 Using tweezers remove the worn silver seal from its housing in the base body ...

Page 234: ...d Troubleshooting Manual 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 Reconnect the signal and ignition cables to the detector 11 Reset the detector to the required operating conditions ...

Page 235: ...the nature and purity of the gases The gases normally used on the ECD are reported in Table 12 2 Table 12 2 Gases used for ECD Carrier gas Make up gas Capillary Columns Packed Columns Helium Nitrogen Hydrogen Nitrogen Argon Methane 5 10 Nitrogen recommended Argon Methane 5 10 When using helium or hydrogen as a carrier gas with capillary or wide bore columns the detector should be fed with nitrogen...

Page 236: ...ions concerning gas supplies Hydrogen is a potentially dangerous gas Mixed with air it may give rise to an explosive mixture The use of hydrogen requires the operator s extreme caution due to the risks involved For further details concerning hydrogen please refer to Using Hydrogen on page xvii Contamination Detector contamination could be indicated by the following effects in the chromatogram redu...

Page 237: ... gas lines Run a leak test Refer to the Performing a Leak Check Capillary Column Operating Sequence on page 181 for instructions Contaminated collecting electrode Clean the collecting electrode as described in the Clean the Collecting Electrode Operating Sequence on page 226 or replace it Chemically contaminated radioactive source Refer to the notes reported in the ECD Maintenance paragraph on pag...

Page 238: ...pendix B Customer Communication contains contact information for Thermo Fisher Scientific offices and affiliates worldwide Contaminated radioactive source Baseline drift with changing pulse voltage Contaminated collecting electrode Refer to the notes reported in the ECD Maintenance paragraph on page 222 Contact your customer support organization Appendix B Customer Communication contains contact i...

Page 239: ...s Detector Chapter at a Glance Nitrogen Phosphorus Detector NPD 240 NPD Maintenance 242 NPD 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 ...

Page 240: ...Chapter 13 Maintaining a Nitrogen Phosphorus Detector Nitrogen Phosphorus Detector NPD 240 Maintenance and Troubleshooting Manual Nitrogen Phosphorus Detector NPD ...

Page 241: ...t pin 206 016 02 7 Ceramic insulator 302 023 10 8 Collecting electrode 259 011 10 9 Retaining screw 311 060 08 10 TS 2 thermionic source standard 465 002 55 TS 1 thermionic source for ENS mode 465 002 50 11 Jet removing tool 205 019 00 12 Detector base body Chapter 13 Nitrogen Phosphorus Detector NPD Maintaining a Nitrogen Phosphorus Detector Maintenance and Troubleshooting Manual 241 ...

Page 242: ...necessary To properly maintain the Nitrogen Phosphorus Detector you should perform the following sequences cleaning the jet replacing the jet cleaning the collecting electrode replacing the collecting electrode replacing the thermionic source Thermionic source The thermionic source installed in the detector may be removed and replaced with a new one or with a source having different coating NOTE N...

Page 243: ...s 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 Therefore before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix B Reagents Saf...

Page 244: ...xample a NPD installed on the right channel is considered RIGHT DETECTOR NPD Source cur A Off Base temp 300 Off Signal pA 10 2 Polarizer V 3 5 H2 delay time Off H2 2 3 Off Air 70 Off Mkup N2 15 Off 2 Scroll to Base temp and press OFF 3 Scroll subsequently to Source curr H2 Air and Mkup and press OFF 4 Disconnect the signal and ignition polarization cables from the detector 5 Loosen the fixing scre...

Page 245: ...g 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 8 Handling the jet with forceps or tweezers rinse the jet with distilled water then with methanol 9 Place the jet on a paper towel and let it air dry PRECAUTIONS ...

Page 246: ...en 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 12 Reconnect the signal and ignition cables to the detector 13 Reset the detector to the required operating conditions Refer to the relevant chapter of the TRACETM GC Ultra Operating manual for more information ...

Page 247: ...t 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 Therefore before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more inform...

Page 248: ...example a NPD installed on the right channel is considered RIGHT DETECTOR NPD Source cur A Off Base temp 300 Off Signal pA 10 2 Polarizer V 3 5 H2 delay time Off H2 2 3 Off Air 70 Off Mkup N2 15 Off 2 Scroll to Base temp and press OFF 3 Scroll subsequently to Source curr H2 Air and Mkup and press OFF 4 Disconnect the signal and ignition polarization cables from the detector 5 Loosen the fixing scr...

Page 249: ...ning a Nitrogen Phosphorus Detector Maintenance and Troubleshooting Manual 249 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 ...

Page 250: ...ing Manual 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 Refer to the relevant chapter of the TRACETM GC Ultra Operating manual for more information ...

Page 251: ... 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 Therefore before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safe...

Page 252: ...alled on the right channel is considered RIGHT DETECTOR NPD Source cur A Off Base temp 300 Off Signal pA 10 2 Polarizer V 3 5 H2 delay time Off H2 2 3 Off Air 70 Off Mkup N2 15 Off 2 Scroll to Base temp and press OFF 3 Scroll subsequently to Source curr H2 Air and Mkup and press OFF 4 Disconnect the signal and ignition polarization cables from the detector 5 Loosen the fixing screw on the front of...

Page 253: ... Using forceps unscrew and remove the contact pin 9 Using tweezers remove the collecting electrode through the top side of the detector cell 10 Place the collecting electrode in the ultrasonic bath filled with liquid detergent and clean for about five minutes 11 Handling the collecting electrode with forceps or tweezers rinse it using tap water then methanol 12 Place the collecting electrode on a ...

Page 254: ...tenance and Troubleshooting Manual 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 Remount the connector holder assembly verifying the contact efficiency ...

Page 255: ...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 19 Reset the detector to the required operating conditions Refer to the relevant chapter of the TRACETM GC Ultra Operating manual for more information ...

Page 256: ...must be carried out at low temperature to avoid burns Therefore before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS WARNING Before replacing the collecting electrode be sure that The flow of the detector gases has been interrupted The detector has been switched off WARNING When handling organics solvents you must take precautions to avoid health hazards Refer ...

Page 257: ... NPD installed on the right channel is considered RIGHT DETECTOR NPD Source cur A Off Base temp 300 Off Signal pA 10 2 Polarizer V 3 5 H2 delay time Off H2 2 3 Off Air 70 Off Mkup N2 15 Off 2 Scroll to Base temp and press OFF 3 Scroll subsequently to Source curr H2 Air and Mkup and press OFF 4 Disconnect the signal and source cables from the detector 5 Loosen the fixing screw on the front of the d...

Page 258: ...ignal cable by unscrewing the two screws that fix it on the detector cell 8 Using forceps unscrew and remove the contact pin 9 Using forceps or tweezers remove the collecting electrode through the top side of the detector cell 10 Place the new collecting electrode into its housing Ensure the insert hole is perfectly vertically aligned to the hole present on the cell ...

Page 259: ...connector holder assembly verifying the contact efficiency 13 Place the detector cell on the detector base body and tighten the fixing screw 14 Screw the detector cap into its housing 15 Reconnect the signal and ignition cables to the detector 16 Reset the detector to the required operating conditions Refer to the relevant chapter of the TRACETM GC Ultra Operating manual for more information ...

Page 260: ... 55 CAUTION Thermionic sources are fragile Handle them with care Gently remove the plastic tube protecting the source ceramic during shipment Especially avoid any excessive transverse force to the source ceramic Before inserting the new source into the holder check that the PTFE insulator is properly interposed WARNING This operation must be carried out at low temperature to avoid burns Therefore ...

Page 261: ...n the following example a NPD installed on the right channel is considered RIGHT DETECTOR NPD Source cur A Off Base temp 300 Off Signal pA 10 2 Polarizer V 3 5 H2 delay time Off H2 2 3 Off Air 70 Off Mkup N2 15 Off 2 Scroll to Base temp and press OFF 3 Scroll subsequently to Source curr H2 Air and Mkup and press OFF 4 Disconnect the signal and source cables from the detector 5 Loosen the fixing sc...

Page 262: ...nd Troubleshooting Manual 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 Gently replace the thermionic source pushing it in straight 9 Fix the thermionic source into its housing tightening the grub screw ...

Page 263: ...shooting Manual 263 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 Refer to the relevant chapter of the TRACETM GC Ultra Operating manual for more information ...

Page 264: ...onsistent flows are necessary to maintain a constant and stable sensitivity Table 13 2 Gases used for NPD Carrier gas Detector Gas Make up gas Gas Capillary Columns Packed Columns Helium Nitrogen Hydrogen Helium Nitrogen Hydrogen Air Nitrogen Helium Nitrogen is preferred over helium as make up gas due to its lower thermal conductivity Using nitrogen the source requires a lower heating current NOTE...

Page 265: ...rogen Phosphorus Detector Maintenance and Troubleshooting Manual 265 Typical flow rates for detector gases are reported in Table 13 3 Table 13 3 Typical NPD operating conditions Gas Flow rate Hydrogen 2 4 mL min Air 40 80 mL min Make up 10 20 mL min ...

Page 266: ...source Detector response lower than expected Lower source temperature Check the base body temperature and source heating current Air contamination in hydrogen line Turn the source off Increase the hydrogen pressure for 10 20 minutes to purge the hydrogen line Check the line tightness High background level Heating current too high Set the correct operating parameter Hydrogen flow too high Set the c...

Page 267: ...iginal baseline Solvent quenching effect Heating current too low Slightly increase the source heating current Unstable baseline Background current level too high Reduce the source heating current value Hydrogen flow fluctuation Check pressure regulators on hydrogen line Low carbon rejection Hydrogen flow too high Reduce hydrogen flow to the correct operative conditions Table 13 4 NPD Troubleshooti...

Page 268: ......

Page 269: ...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 Replace the Interferential Filter 297 Replace the Heat Shields 301 ...

Page 270: ...r 14 Maintaining a Flame Photometric Detector Flame Photometric Detector FPD 270 Maintenance and Troubleshooting Manual Flame Photometric Detector FPD 1 2A 3 5 4 7 2B 2C 8 9 2D 2E 15 10 11 12 13 14 2F 17 16 6 ...

Page 271: ...um O ring 290 326 30 7 Jet 404 045 11 8 Spacer 9 Flange 10 Filter support 11 Interferential filter for phosphorus 281 071 00 Interferential filter for sulphur 281 070 00 Interferential filter for tin 281 070 01 12 Photomultiplier assembly 13 Signal cable 14 Excitation voltage cable 15 Ignition heating multipolar cable 16 FPD fixing tool 205 021 50 17 5 mm wrench for jet Chapter 14 Flame Photometri...

Page 272: ...st 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 cleaning the jet cleaning the interferential filter cleaning the mirror metal plug cleaning the flame side heat shield replacing the jet replacing the interferential filter replacing the heat s...

Page 273: ...Ultrasonic cleaning bath Liquid detergent Clean compressed air GC grade methanol Paper towels 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 PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Inf...

Page 274: ...PD Flame Off Base temp 300 Off FPD temp 150 Off Signal pA xx High voltage mode N H2 90 Off Air 115 Off Mkup N2 0 0 2 Scroll to Flame and press OFF 3 Scroll subsequently to Base temp FPD temp H2 and Air and press OFF 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...

Page 275: ...se the aluminium ring inserted between the detector head and the base body 7 Using the 5 mm wrench provided with the GC loosen the jet and remove it from the detector base body 8 Place the jet in the ultrasonic bath filled with liquid detergent and clean it for about five minutes 9 Handling the jet with forceps or tweezers rinse the jet with distilled water then with methanol 10 Place the jet on a...

Page 276: ... Maintenance and Troubleshooting Manual 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 ...

Page 277: ...e and Troubleshooting Manual 277 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 TRACETM GC Ultra Operating manual for more information ...

Page 278: ...o room temperature PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more information 1 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the FPD detector to access the FPD control table In the following example a FPD installed on the right channel is considered RIGHT DET FPD Fl...

Page 279: ...ing Manual 279 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 5 Disconnect the signal excitation voltage and ignition heating cables from the detector ...

Page 280: ...voltage On Make sure the GC power supply has been switched off before disconnecting the tube from the detector body 7 Remove the interferential filter from its housing handling it very gently Keep it using a clean paper towel CAUTION Filters are fragile Pay attention not to let the filter fall down and damage 8 Using a clean paper towel clean the filter on both faces CAUTION Avoid touching the fil...

Page 281: ...must be oriented towards the flame 10 Reassembly the photomultiplier tube and the detector body then fix them together tightening the knurled nut 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 TRACETM GC Ultra Operating manual for more information ...

Page 282: ... 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 Therefore before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more ...

Page 283: ...T DET FPD Flame Off Base temp 300 Off FPD temp 150 Off Signal pA xx High voltage mode N H2 90 Off Air 115 Off Mkup N2 0 0 2 Scroll to Flame and press OFF 3 Scroll subsequently to Base temp FPD temp H2 and Air and press OFF 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 sho...

Page 284: ...detector and remove it CAUTION Pay attention not to lose the aluminium ring inserted between the detector head and the base body 7 Loosen the Allen screws on the mirror plug and remove it 8 Using a clean paper towel clean the mirror surface of the plug If necessary use a solvent as methylene chloride or methanol to remove deposits and a metal polishing paste to restore it to the previous reflectiv...

Page 285: ... fix it with the relevant Allen screws NOTE Before reinserting the plug inspect the graphite seal inside the plug s housing If the seal is damaged and could not ensure tightness it must be removed and replaced with a new one 10 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 ...

Page 286: ... Maintenance and Troubleshooting Manual 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 TRACETM GC Ultra Operating manual for more information ...

Page 287: ... 205 021 50 1 mm Allen wrench Cotton sticks Paper towels Methylene chloride or 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 PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Informati...

Page 288: ...IGHT DET FPD Flame Off Base temp 300 Off FPD temp 150 Off Signal pA xx High voltage mode N H2 90 Off Air 115 Off Mkup N2 0 0 2 Scroll to Flame and press OFF 3 Scroll subsequently to Base temp FPD temp H2 and Air and press OFF 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 ...

Page 289: ...osen the Allen screws on the mirror plug and remove it 8 With the aid of a cotton stick clear the surface of the heat shield that faces the flame If necessary use a solvent like methylene chloride or methanol to help cleaning the heat shield CAUTION While cleaning the heat shield pay attention not to damage the ignition coil 9 Using a clean paper towel clean the mirror surface of the plug If neces...

Page 290: ...and fix it with the relevant Allen screws NOTE Before reinserting the plug inspect the graphite seal inside the plug s housing If the seal is damaged and could not ensure tightness it must be removed and replaced with a new one 11 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 ...

Page 291: ...aintenance and Troubleshooting Manual 291 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 TRACETM GC Ultra Operating manual for more information ...

Page 292: ...erefore before beginning the sequence the detector must be cooled to room temperature PRECAUTIONS 1 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the FPD detector to access the FPD control table In the following example a FPD installed on the right channel is considered RIGHT DET FPD Flame Off Base temp 300 Off FPD temp 150 Off Signal pA xx High voltage mode N H2 90 Off Air 11...

Page 293: ...al 293 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 5 Disconnect the signal excitation voltage and ignition heating cables from the detector ...

Page 294: ... 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 7 Using the 5 mm wrench provided with the GC loosen the worn jet and remove it from the detector base body ...

Page 295: ...tric Detector Maintenance and Troubleshooting Manual 295 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 ...

Page 296: ...enance and Troubleshooting Manual 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 TRACETM GC Ultra Operating manual for more information ...

Page 297: ... 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 Target compound P N Phosphorus 281 071 00 Sulphur 281 070 00 Organotin 281 070 01 detector 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 tempera...

Page 298: ...IGHT DET FPD Flame Off Base temp 300 Off FPD temp 150 Off Signal pA xx High voltage mode N H2 90 Off Air 115 Off Mkup N2 0 0 2 Scroll to Flame and press OFF 3 Scroll subsequently to Base temp FPD temp H2 and Air and press OFF 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 ...

Page 299: ...ient light with the excitation voltage set to On Make sure the GC power supply has been switched off before disconnecting the tube from the detector body 7 Remove the interferential filter from its housing handling it very gently Keep it using a clean paper towel CAUTION Filters are fragile Pay attention not to let the filter fall down and damage Avoid touching the filter with your fingers If you ...

Page 300: ...ust be oriented towards the flame 9 Reassembly the photomultiplier tube and the detector body then fix them together tightening the knurled nut 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 TRACETM GC Ultra Operating manual for more information ...

Page 301: ...ce kit P N 190 045 89 1 mm Allen wrench Screwdriver Methylene chloride or methanol Paper towels 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 PRECAUTIONS WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety I...

Page 302: ...IGHT DET FPD Flame Off Base temp 300 Off FPD temp 150 Off Signal pA xx High voltage mode N H2 90 Off Air 115 Off Mkup N2 0 0 2 Scroll to Flame and press OFF 3 Scroll subsequently to Base temp H2 and Air and press OFF 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 an...

Page 303: ...y 7 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 On Make sure the GC power supply has been switched off before disconnecting the tube from the detector body 8 Remove the interferential filter from its housing handling it very gently Keep it...

Page 304: ...and let the filter side heat shield come out from the flange Pay attention not to lose the O ring inserted in the filter support 11 If you want to replace only the filter side heat shield go to 21 If you want to replace the flame side heat shield loosen the three Allen screws that fix the flange to the detector body and remove it with the spacer that should remain inserted in the flange Now you co...

Page 305: ...ewdriver or other unsharpened tool in the combustion chamber and push the flame side heat shield and its graphite seal out from its housing Act gently to avoid breaking of the heat shield CAUTION While pushing out the heat shield pay attention not to damage the ignition coil 14 Remove with care traces of graphite due to the breaking of the seal 15 Insert a new heat shield into its housing inside t...

Page 306: ...m 17 Insert a new graphite seal on the spacer pushing it slowly until it touches the flange 18 Insert the flange into the detector body and fix it tightening the three Allen screws 19 Using a clean paper towel clean the mirror surface of the plug If necessary use a solvent as methylene chloride or methanol to remove deposits and a metal polishing paste to restore it to the previous reflectivity ...

Page 307: ...OTE Before reinserting the plug inspect the graphite seal inside the plug s housing If the seal is damaged and could not ensure tightness remove it and replace with a new one 21 Insert a new heat shield into its housing inside the flange 22 Insert the filter support into the flange and fix it tightening the three Allen screws Check the O ring that fixes the heat shield is in place before tightenin...

Page 308: ...o 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 24 Reassembly the photomultiplier tube and the detector body then fix them together tightening the knurled nut ...

Page 309: ...y 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 27 Switch on the GC power supply and set the detector to the required operating conditions Refer to the TRACETM GC Ultra Operating manual for more information ...

Page 310: ... described in the maintenance sequences to avoid reducing sensitivity Replace the heat shields if the deposits due to contamination cannot be eliminated Gases A right choice of the flow rates of hydrogen and air fuel gases is of primary importance in determining FPD sensitivity Flow rates will affect also selectivity and to a great extent peak shapes Optimum carrier gas flow rate depends on the ty...

Page 311: ...ptimum air flow rate should be found experimentally setting a proper value for the hydrogen and performing some analyses on a standard mixture at different air flow rates WARNING It is the customer s responsibility to ensure compliance with all local safety regulations concerning gas supplies Hydrogen is a potentially dangerous gas Mixed with air it may give rise to an explosive mixture The use of...

Page 312: ...g Check the interferential filter has been correctly installed No standing current Signal or power cables incorrectly connected Check connections Faulty photomultiplier tube Contact your customer support organization Refer to Appendix B Customer Communication for contact information Unstable and excessively noisy baseline Faulty photomultiplier tube Contact your customer support organization Refer...

Page 313: ...Interferential Filter Operating Sequence on page 278 The mirror of the combustion chamber is dirty Clean the mirror Refer to Clean the Mirror Metal Plug Operating Sequence on page 282 The flame side heat shield is dirty Clean the flame side heat shield Refer to Clean the Flame side Heat Shield Operating Sequence on page 287 Reduced transparency of the heat shields Replace the heat shields Refer to...

Page 314: ......

Page 315: ...al 315 15 Maintaining a Photoionization Detector Chapter at a Glance Photoionization Detector PID 316 PID Maintenance 318 PID Troubleshooting 334 Operating Sequences Replace the UV Lamp 319 Clean the Lamp Window 323 Checking for Leaks 328 ...

Page 316: ...Chapter 15 Maintaining a Photoionization Detector Photoionization Detector PID 316 Maintenance and Troubleshooting Manual Photoionization Detector PID ...

Page 317: ...31 00 7 Lamp housing 8 VitonTM O ring for lamp holder 290 203 25 9 Heat sink 10 UV lamp 8 4 eV 305 030 13 UV lamp 9 6 eV 305 030 14 UV lamp 10 6 eV 305 030 15 UV lamp 11 8 eV 305 030 16 11 VitonTM O ring for UV lamp 290 203 38 12 Lamp holder 13 Capillary adapter 350 438 25 14 Silver seal 290 150 59 Chapter 15 Photoionization Detector PID Maintaining a Photoionization Detector Maintenance and Troub...

Page 318: ...atic compounds 9 6 eV Determination of low boiling aromatic compounds BTEX analyses 10 6 eV General applications Filled with krypton emits at 10 0 and 10 6 eV 11 8 eV Determination of aldehydes and ketones Available UV lamps for PID detection NOTE Keep always a spare UV lamp in your laboratory because the lamp could collapse suddenly without warning signs CAUTION Make sure to have appropriate filt...

Page 319: ... for UV lamp P N 290 203 38 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 PRECAUTIONS WARNING The lamp replacement can be carried out at operating temperature without removing the detector from its base body Nevertheless keep in mind that parts of the detector are hot and could cause injuries t...

Page 320: ...f the PID detector to access the PID control table In the following example a PID installed on the right channel is considered RIGHT DET PID Lamp Off Base temp 250 250 High current N Signal pA xx Mkup N2 7 Off Sheath gas 40 Off 2 Scroll subsequently to Lamp Mkup and Sheath gas and press OFF 3 Loosen the two knurled screws that fix the lamp holder to the lamp housing and remove it ...

Page 321: ... 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 5 Place the proper VitonTM O ring on the new lamp so to contact its flange 6 Insert the lamp into the holder pushing it in until it stops CAUTION While inserting the lamp pay attention not to damage the contact pin inside the holder ...

Page 322: ...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 RIGHT DETECTOR PID control table scroll subsequently to Mkup Sheath Gas and Lamp and press ON CAUTION Before starting a new analysis wait about 30 minutes so the lamp output can stabilize ...

Page 323: ...injuries to your eyes Therefore before beginning the sequence make sure the UV lamp has been switched off PRECAUTIONS WARNING The cleaning of the lamp window can be carried out without removing the detector from its base body Nevertheless keep in mind that parts of the detector are hot and could cause injuries to your hands PRECAUTIONS WARNING When handling organics solvents you must take precauti...

Page 324: ... of the PID detector to access the PID control table In the following example a PID installed on the right channel is considered RIGHT DET PID Lamp Off Base temp 250 250 High current N Signal pA xx Mkup N2 7 Off Sheath gas 40 Off 2 Scroll subsequently to Lamp Mkup and Sheath Gas press OFF 3 Loosen the two knurled screws that fix the lamp holder and remove it from the lamp housing ...

Page 325: ...the lamp 6 Wet the cotton tip of the applicator included in the lamp polishing kit with tap water and dip it into the polishing powder so to pick up a small amount of it 7 Swab the lamp window in a circular motion until the UV absorbing film deposited on its surface has been removed CAUTION Apply only a light pressure on the applicator while polishing the window Heavy pressure could cause abrasion...

Page 326: ...with GC grade methanol or acetone 10 Wipe the window using a clean paper towel 11 Air dry the lamp 12 Insert the VitonTM O ring on the lamp pushing it in until it touches the flange 13 Insert the lamp into the holder pushing it in until it stops CAUTION While inserting the lamp pay attention not to damage the contact pin inside the holder ...

Page 327: ...tor Maintenance and Troubleshooting Manual 327 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 RIGHT DETECTOR PID control table scroll subsequently to Mkup Sheath Gas and Lamp and press ON ...

Page 328: ...ing the operation make sure the UV lamp has been switched off PRECAUTIONS WARNING This operation must be carried out at low temperature to avoid burns Therefore before beginning the procedure the detector must be cooled to room temperature PRECAUTIONS 1 Insert the end of the exit line into a piece of silicon rubber disconnecting it from the base body of the second detector if any 2 Close the purge...

Page 329: ...ll to Pressure and set 200 6 XXX DET PID Lamp Off Base temp 250 250 High current N Signal pA xx Mkup N2 30 Off Sheath gas 40 200 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the PID detector to access the PID control table 7 Set Lamp to Off 8 Set Mkup N2 to Off 9 Set Sheath gas to 200 10 Wait some minutes until the pressure in the system is equilibrated 11 XXX DET PID Lamp Of...

Page 330: ... if the pressure begins to drop immediately one or more leaks are present 13 Using the leak detector check the connection between the capillary adapter and the detector located inside the oven 14 If a leak is detected replace the seal of the capillary adapter 14 in the exploded view reported on page 316 In this case repeat the leak test to ensure complete tightness 15 If the detector localizes the...

Page 331: ...for Leaks Maintaining a Photoionization Detector Maintenance and Troubleshooting Manual 331 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 ...

Page 332: ...a Photoionization Detector Checking for Leaks 332 Maintenance and Troubleshooting Manual 18 Remove the heat sink 19 Tighten the detector cell using the fixing tool provided 20 Reassemble the detector and repeat the leak test ...

Page 333: ...or Maintenance and Troubleshooting Manual 333 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 ...

Page 334: ...Operation Sequence on page 319 Contamination An abnormally high baseline may indicate contamination of the detector In this case turning off the lamp will not make the symptom disappear This means that the detector cell has been contaminated Try to solve the problem by baking the cell for two hours at 400 C If the symptom does not disappear contact your customer support organization Refer to Appen...

Page 335: ...der Reinstall the UV lamp Refer to the Replace the UV Lamp Operating Sequence on page 319 Lamp holder not correctly fixed to the lamp housing Tighten the two knurled screws that fix the lamp holder to the housing Lamp power cable disconnected Check the connection Polarization cable disconnected Check the connection Safety interlock circuit is faulty Contact your customer support organization Refer...

Page 336: ...C If the symptom does not disappears contact your customer support organization Refer to Appendix B Customer Communication for contact information Inadequate gas flow rate settings Set gas flow rates to proper values Leaks on the gas lines Perform a leak test Refer to the Performing a Leak Check Capillary Column on page 181 Low sensitivity Lamp window fogged by UV absorbing deposits Clean the lamp...

Page 337: ...Maintenance and Troubleshooting Manual 337 16 Maintaining a Thermal Conductivity Detector Chapter at a Glance Thermal Conductivity Detector TCD 338 TCD Maintenance 340 TCD Troubleshooting 341 ...

Page 338: ...Chapter 16 Maintaining a Thermal Conductivity Detector Thermal Conductivity Detector TCD 338 Maintenance and Troubleshooting Manual Thermal Conductivity Detector TCD 10 11 12 13 9 1 4 3 2 6 7 8 5 ...

Page 339: ...ing 8 Fixing nut 9 Kit for connecting capillary columns 347 095 42 10 Retaining nut for 6 mm OD column and ferrule 350 201 17 11 Retaining nut for 4 mm OD column and ferrule 350 201 18 12 Knurled nut O ring and washer for 6 mm OD glass column 350 201 19 13 Nut ferrule and washer for 6 mm OD glass column 350 201 22 Chapter 16 Thermal Conductivity Detector TCD Maintaining a Thermal Conductivity Dete...

Page 340: ...the filaments lifetime Avoid injecting samples that contain halogenated or acid compounds at high concentrations Ensure that oxygen air could not enter into the filaments cells Oxidation would irreversibly damage the filaments Install traps for moisture and oxy gen on the gas lines to reduce the hazard WARNING Set Filament power to Off before disconnecting the column from the detector When the col...

Page 341: ...lecular weight compounds inside the cell or to contaminated gases Low temperatures of the detector block may cause high boiling compounds condensate on the filaments reducing sensitivity Baseline drift A small baseline drift normally occurs during a temperature program and does not indicate a trouble This effect is due to the decrease of the carrier gas flow rate as temperature increases A baselin...

Page 342: ... Refer to the TRACETM GC Ultra Operating Manual for instructions Trans temp set too high Set Trans temp to a proper value about 10 to 20 C below the Block temp value Faulty temperature regulation Contact your customer support organization Refer to Appendix B Customer Communication for contact information Baseline drift Unstable regulation of the flow rate of the gases Check the controllers of the ...

Page 343: ... Constant Temperature Refer to the TRACE GC Ultra Operating Manual for instructions Thermal conductivity of the carrier gas is too close to the one of the compound to be analyzed Use a different carrier gas Refer to the TRACE GC Ultra Operating Manual for instructions Contaminated filaments Remove contamination by baking the filaments for one hour at a temperature higher than the boiling point of ...

Page 344: ...tion Low sensitivity Oxidized filaments Contact your customer support organization Refer to Appendix B Customer Communication for contact information The detector does not work Message Filament power Off Lack of carrier make up or reference gas or pressure too low Check the feed of the carrier make up and reference gas Filament burnt Contact your customer support organization Refer to Appendix B C...

Page 345: ...es 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 Replace the Silver Seal FID on ECD 369 Replace the Silver Seal NPD on ECD 375 Replace the Silver Seal FPD on ECD 381 ...

Page 346: ...Chapter 17 Maintaining Detectors in Stack Configuration ECD adapted for Stack Configuration 346 Maintenance and Troubleshooting Manual ECD adapted for Stack Configuration 1 8 12 5 6 11 2 3 4 9 10 7 ...

Page 347: ...nector 5 Detector adapter 347 090 07 6 Heating block 354 250 64 7 Heat shield 241 044 49 8 Collecting electrode 277 003 50 9 Silver seal 290 150 58 10 Temperature sensor heater assembly 190 500 87 11 ECD fixing tool 205 021 50 12 Seal 290 326 08 Chapter 17 ECD adapted for Stack Configuration Maintaining Detectors in Stack Configuration Maintenance and Troubleshooting Manual 347 ...

Page 348: ...ph You will find instructions in the relevant chapters of this manual In this chapter you will find instructions on how to perform ECD maintenance when installed in stack configuration respectively with a FID NPD and FPD detector To properly maintain the ECD you should perform the following cleaning or replacement sequences cleaning the collecting electrode replacing the collecting electrode repla...

Page 349: ...e Fine emery paper optional WARNING Any maintenance or repair operations involving the radioactive source of the ECD must be performed ONLY by qualified personnel duly authorized to handle radioactive material Please contact your local Thermo Fisher Scientific Technical Service office WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reag...

Page 350: ...A 5 4 Ign tresh 2 0 Flameout retry Off H2 35 Off Air 350 Off In the AUX DETECTOR FID table scroll to Flame and press OFF 4 Scroll subsequently to Base temp H2 and Air and press OFF 5 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the ECD to access the ECD control table XXX DETECTOR ECD Base temp 250 Off ECD temp 250 Off Ref current nA 1 0 Freq kHz 2 15 Pulse amp V 25 Pulse widt...

Page 351: ... Detectors in Stack Configuration Maintenance and Troubleshooting Manual 351 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 ...

Page 352: ...ctrode FID on ECD 352 Maintenance and Troubleshooting Manual 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 Use a 3 mm Allen wrench ...

Page 353: ...4 Unscrew the collecting electrode and remove it using tweezers 15 If you are going to replace the collecting electrode with a new one go to step 16 If you are going to clean it put it into an ultrasonic bath filled with a toluene hexane mixture and sonicate it In the most critical cases fine emery paper can be used 16 Mount the new or cleaned electrode without touching it Use tweezers 17 Remount ...

Page 354: ...Collecting Electrode FID on ECD 354 Maintenance and Troubleshooting Manual 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 Remount the FID detector on the top of the ECD and tighten the fixing screw ...

Page 355: ...d 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 23 Press AUX 24 Scroll to Detector and press ENTER 25 In the AUX DETECTOR FID table reset the auxiliary FID detector to the required operating conditions ...

Page 356: ...e Fine emery paper optional WARNING Any maintenance or repair operations involving the radioactive source of the ECD must be performed ONLY by qualified personnel duly authorized to handle radioactive material Please contact your local Thermo Fisher Scientific Technical Service office WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reag...

Page 357: ...nal pA 10 2 Polarizer V 3 5 H2 delay time Off H2 2 2 Air 60 60 In the AUX DETECTOR NPD table scroll to Base temp and press OFF 4 Scroll subsequently to Source curr H2 Air and press OFF 5 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the ECD to access the ECD control table XXX DETECTOR ECD Base temp 250 Off ECD temp 250 Off Ref current nA 1 0 Freq kHz 2 15 Pulse amp V 25 Pulse ...

Page 358: ...e Collecting Electrode NPD on ECD 358 Maintenance and Troubleshooting Manual 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 ...

Page 359: ...tors in Stack Configuration Maintenance and Troubleshooting Manual 359 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 Use a 3 mm Allen wrench ...

Page 360: ... 14 Unscrew the collecting electrode and remove it using tweezers 15 If you are going to replace the collecting electrode with a new one go to step 16 If you are going to clean it put it into an ultrasonic bath filled with a toluene hexane mixture and sonicate it In the most critical cases fine emery paper can be used 16 Mount the new or cleaned electrode without touching it Use tweezers 17 Remoun...

Page 361: ...etectors in Stack Configuration Maintenance and Troubleshooting Manual 361 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 Remount the NPD detector on the top of the ECD and tighten the fixing screw ...

Page 362: ...d 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 23 Press AUX 24 Scroll to Detector and press ENTER 25 In the AUX DETECTOR NPD table reset the auxiliary NPD detector to the required operating conditions ...

Page 363: ...lecting electrode P N 277 003 50 for cleaning Ultrasonic cleaning bath GC grade hexane GC grade toluene Fine emery paper optional WARNING Any maintenance or repair operations involving the radioactive source of the ECD must be performed ONLY by qualified personnel duly authorized to handle radioactive material Please contact your local Thermo Fisher Scientific Technical Service office WARNING This...

Page 364: ...f the GC power supply is imperative to avoid electrical shocks and damages to the instrument WARNING When handling organics solvents you must take precautions to avoid health hazards Refer to Appendix A Reagents Safety Information for more information 1 Switch off the GC power supply and wait until the detectors have cooled to room temperature 2 Disconnect the signal excitation voltage and ignitio...

Page 365: ...ce and Troubleshooting Manual 365 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 4 Disconnect the signal excitation and heater cables from the ECD detector ...

Page 366: ...ch 6 Unscrew the collecting electrode and remove it using tweezers 7 If you are going to replace the collecting electrode with a new one go to step 8 If you are going to clean it put it into an ultrasonic bath filled with a toluene hexane mixture and sonicate it In the most critical cases fine emery paper can be used 8 Mount the new or cleaned electrode without touching it Use tweezers 9 Remount t...

Page 367: ...ual 367 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 11 Reconnect the excitation and heater cables to the ECD detector 12 Reconnect the signal excitation voltage and ignition heating cables to the FPD 13 Switch on the GC power supply ...

Page 368: ...68 Maintenance and Troubleshooting Manual 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 16 Scroll to Detector and press ENTER 17 In the AUX DETECTORS table set the FPD detector to the required operating conditions ...

Page 369: ...erations involving the radioactive source of the ECD must be performed ONLY by qualified personnel duly authorized to handle radioactive material Please contact your local Thermo Fisher Scientific Technical Service office WARNING This operation must be carried out at low temperature to avoid burns Therefore before beginning the sequence the detectors must be cooled to room temperature PRECAUTIONS ...

Page 370: ...the AUX DETECTOR FID table scroll to Flame and press OFF 4 Scroll subsequently to Base temp H2 and Air and press OFF 5 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the ECD to access the ECD control table XXX DETECTOR ECD Base temp 250 Off ECD temp 250 Off Ref current nA 1 0 Freq kHz 2 15 Pulse amp V 25 Pulse width us 1 0 Mkup N2 40 Off 6 Scroll subsequently to Base temp and E...

Page 371: ...g Manual 371 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 ...

Page 372: ...ck Configuration Replace the Silver Seal FID on ECD 372 Maintenance and Troubleshooting Manual 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 ...

Page 373: ...figuration Maintenance and Troubleshooting Manual 373 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 Reconnect the signal and ignition polarization cables to the FID ...

Page 374: ...nce and Troubleshooting Manual 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 18 Scroll to Detector and press ENTER 19 In the AUX DETECTOR FID table set the FID detector to the required operating conditions ...

Page 375: ...erations involving the radioactive source of the ECD must be performed ONLY by qualified personnel duly authorized to handle radioactive material Please contact your local Thermo Fisher Scientific Technical Service office WARNING This operation must be carried out at low temperature to avoid burns Therefore before beginning the sequence the detectors must be cooled to room temperature PRECAUTIONS ...

Page 376: ...In the AUX DETECTOR NPD table scroll to Base temp and press OFF 4 Scroll subsequently to Source curr H2 Air and press OFF 5 Press LEFT DETECTOR or RIGHT DETECTOR depending on the location of the ECD to access the ECD control table XXX DETECTOR ECD Base temp 250 Off ECD temp 250 Off Ref current nA 1 0 Freq kHz 2 15 Pulse amp V 25 Pulse width us 1 0 Mkup N2 40 Off 6 Scroll subsequently to Base temp ...

Page 377: ...g Manual 377 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 ...

Page 378: ...ck Configuration Replace the Silver Seal NPD on ECD 378 Maintenance and Troubleshooting Manual 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 ...

Page 379: ...figuration Maintenance and Troubleshooting Manual 379 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 Reconnect the signal and ignition polarization cables to the NPD ...

Page 380: ...nce and Troubleshooting Manual 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 18 Scroll to Detector and press ENTER 19 In the AUX DETECTOR NPD table set the NPD detector to the required operating conditions ...

Page 381: ...alified personnel duly authorized to handle radioactive material Please contact your local Thermo Fisher Scientific Technical Service office WARNING This operation must be carried out at low temperature to avoid burns Therefore before beginning the sequence the detectors must be cooled to room temperature PRECAUTIONS WARNING Before disconnecting the cables or disassembling an FPD detector switchin...

Page 382: ...l 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 ...

Page 383: ... on ECD Maintaining Detectors in Stack Configuration Maintenance and Troubleshooting Manual 383 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 ...

Page 384: ...ntenance and Troubleshooting Manual 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 Reconnect the signal and ignition polarization cables to the FPD 10 Switch on the GC power supply ...

Page 385: ...e and Troubleshooting Manual 385 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 13 Scroll to Detector and press ENTER 14 In the AUX DETECTORS table set the FPD detector to the required operating conditions ...

Page 386: ...anual 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 installation of the column inside the ECD To correct the symptom reinstall the column and check it for leaks To ensure a right insertion of the column inside the detector base body the distance be...

Page 387: ... 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 ...

Page 388: ...ine and an external oven to keep the filter at the regeneration temperature If an external oven is not present in your lab the column oven of the GC should be use Before starting the following preliminary operations must be carried out Cool the oven and detector base body to room temperature Close the gas supplies Turn off the main power on the rear panel of the GC Disconnect the main power cable ...

Page 389: ...GC Ultra Top Cover Removing Active Carbon Filter 1 Use the appropriate wrench the loosen each retaining nut CARRIER SPLIT PURGE 1 2 2 3 3 4 5 2 2 3 3 4 2 1 Carrier Gas Line Filter 3 2 M6x0 75 mm Retaining Nut 4 3 1 6 mm OD Aluminium Ferrule 5 4 Arrow indicating the Flow Direction 6 5 Split Line Filter 7 8 Finger loosen the retaining nuts of the filter to regenerate ...

Page 390: ...next figure Gas flow direction 1 2 3 4 5 11 1 External Nitrogen Line 12 2 M6x0 75 mm Retaining Nut 13 3 1 6 mm OD Aluminium Ferrule 14 4 Active Carbon Filter 15 5 Arrow indicating the Flow Direction 16 17 Set a supply gas pressure of 0 5 bar to obtain a flow of at least 100 mL min 18 Place the filter into an external oven or into the column oven of the GC Keep the filter at a temperature of 300 C ...

Page 391: ...hooting Manual 391 19 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 ...

Page 392: ...els in the gas source Use correct gas purity Drifting Falling Carrier gas leak in the system Perform a leak test and ensure the tightness of the connections on the carrier gas line Column is baking out Allow enough time for the column to stabilize Rising Accumulation of impurities in column Check impurity levels in the gas source Use correct gas purity Contaminated detector Check the detector and ...

Page 393: ...he upper column temperature Bake out the column Install a high temperature column Oxygen contamination is decomposing the stationary phase Install oxygen filters in carrier gas line Check pneumatic and inlet systems for leaks Use correct gas purity with low oxygen content Square waves Large AC power fluctuations heavy equipment on same line Use a dedicated clean AC line of sufficient amperage Nois...

Page 394: ...lumn fittings Tighten fittings accordingly Loose detector electrical connections Make sure the leads are properly connected Spiking Defective electrometer or amplifier Replace the electrometer or amplifier F s column too close to flame FID Lower the column to the correct position 2 3 mm below the tip of the jet Dirty jet or detector Isolate the detector from the electronics If noise disappears cle...

Page 395: ...y phase accumulated in the outlet Remove the last two coils from the column Detector base body temperature too low Increase the temperature to 5 C below the column maximum Clipping at bottom Detector or integrator zero set too low Set the zero correctly at top Data system zoomed in too close Zoom out to view the entire chromatogram Detector or integrator attenuation set too low Set the attenuation...

Page 396: ...ected sample Decrease the injection port temperature Use the on column injection technique Dirty injection solution Carry out adequate clean up of sample prior to injection Ghost peaks Broad ghost peaks Contaminated inlet or pneumatics Remove the column and bake out the inlet Use a high quality septum Replace the split vent filter Install an in line filter between the pneumatics and the inlet Inco...

Page 397: ...e column position No peaks at all Clogged syringe needle Replace or repair the syringe Column broken or disconnected Check the column and connections Defective electrometer or amplifier Replace the electrometer or amplifier Defective recording device Replace the recording device FID flame is out Light the flame Poor or missing electrical connection Check the cable connections Incorrect column posi...

Page 398: ...e Tailing Solvent peak Incorrect column position in inlet Reinstall the column Initial oven temperature too high On Column Reduce the initial oven temperature Septum purge flow too low and or split splitless vent flow too low Check and adjust the septum purge and vent flows Too large injection size Reduce the injection size Unresolved peaks Carrier gas flow rate too high Reduce the carrier gas flo...

Page 399: ...s Non reproducible sample injection technique Evaluate the sample preparation sequences Compare the results with a series of standard injections Leaking syringe or septum Check and replace the syringe and or septum at regular intervals Leaks at the injection Check the column connections Run a leak check Poor injection technique Carefully meter the injected amount Use a clean good quality syringe P...

Page 400: ...y oxygen and or water Use a carrier gas free of oxygen and water Stationary phase loss due to column bleeding Reduce the column temperature Increasing Increasing carrier leakage Check the septum and column connections Carrier gas supply running out Replace the bottle Low reproducibility Drifting or unstable pneumatic controller Monitor the column pressure or flow Check and replace the controller i...

Page 401: ... 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 Use http www thermo com com cda resources resource_detail 1 12512 00 html address for products information Use http www gc gcms customersupport com WebPage Share Default aspx address to contact your local Thermo Fisher Scientific office o...

Page 402: ...e complete 1 2 3 4 5 The technical information is easy to understand 1 2 3 4 5 Examples of operation are clear and useful 1 2 3 4 5 The figures are helpful 1 2 3 4 5 I was able to install the system using this manual 1 2 3 4 5 If you would like to make additional comments please do Attach additional sheets if necessary _______________________________________________________________________________...

Page 403: ... 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 The following are the chemical references of the solvents mentioned in this manual ACETONE ACETONE 2 Propanone Dimethyl ketone C3H6O CH3 CO CH3 Molecular mass 58 1 CAS 67 64 1 RTECS AL3150000...

Page 404: ... METHANOL METHANOL Methyl alcohol Carbinol Wood alcohol CH4O CH3OH Molecular mass 32 0 CAS 67 56 1 RTECS PC1400000 ICSC 0057 UN 1230 EC 603 001 00 X TOLUENE TOLUENE Methyl benzene Toluol C6H5CH3 C7H8 Molecular mass 92 1 CAS 108 88 3 RTECS XS5250000 ICSC 0078 UN 1294 EC 601 021 00 3 ...

Page 405: ...ions acronyms metric prefixes and symbols A A ampere ac alternating current ADC analog to digital converter B b bit B byte 8 b baud rate data transmission speed in events per second C ºC Celsius CIP Carriage and Insurance Paid To cm centimeter CPU central processing unit of a computer CSE Customer Service Engineer D d depth DAC digital to analog converter dc direct current DS data system ...

Page 406: ...e on Board FPD Flame Photometric Detector ft foot G g gram gain A measure of the ability of an electronic circuit or device to increase the magnitude of an electronic input parameter GC gas chromatograph GND electrical ground H h height h hour harmonic distortion A high frequency disturbance that appears as distortion of the fundamental sine wave HOT OC High Oven Temperature Cold On Column Injecto...

Page 407: ...ide diameter IEC International Electrotechnical Commission impulse See transient in inch I O input output K k kilo 103 or 1024 K Kelvin kg kilogram kPa kilopascal L l length l liter LAN Local Area Network lb pound LED light emitting diode LVOCI Large Volume On Column Injector LVSL Large Volume Injector M ...

Page 408: ...scus The curved upper surface of a column of liquid min minute mL milliliter mm millimeter m z mass to charge ratio N n nano 10 9 negative polarity The inverse of a detector signal polarity nm nanometer NPD Nitrogen Phosphorous Detector O OCI On Column Injector OD outside diameter ohm P p pico 10 12 Pa pascal PCB printed circuit board ...

Page 409: ... access memory RF radio frequency ROM read only memory RS 232 industry standard for serial communications S s second S SL Split Splitless Injector sag See surge slow average A gradual long term change in average RMS voltage level with typical durations greater than 2 s SOP Standard Operating Procedures source current The current needed to ignite a source such as a detector lamp surge A sudden chan...

Page 410: ...ent with the denominator For example C min 1 instead of C min g L 1 instead of g L TCD Thermal Conductivity Detector transient A brief voltage surge of up to several thousand volts with a duration of less than 50 µs U UFM Ultra Fast Module V V volt V ac volts alternating current V dc volts direct current VGA Video Graphics Array W w Width W Watt ...

Page 411: ...lace the Liner 151 Replace a Broken Liner 157 Adjust a Quartz Wool Packing 165 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 Clean the Jet 195 Replace the Jet 199 Clean the Collecting Electrode 202 Replace the Collecting Electrode 207 Replace the Ignition Assembly 211 Clean the Collecting...

Page 412: ...n 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 Replace the Silver Seal FID on ECD 369 Replace the Silver Seal NPD on ECD 375 Replace the Silver Seal FPD on ECD 381 To Regenerate Carrier Gas and Split Lines Filters 388 ...

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