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14 Maintaining the ECD

Exploded Parts View of the Electron Capture Detector

232

Maintaining Your GC

Exploded Parts View of the Electron Capture
Detector

Figure 47.

Electron Capture Detector (ECD) exploded parts

Column nut

Makeup gas adapter

Liner

Cap

Adapter nut

Ferrules

Warning tag

Electrometer

Perforated cover

Makeup gas line

Summary of Contents for 8890

Page 1: ...Agilent 8890 Gas Chromatograph Maintaining Your Gas Chromatograph GC ...

Page 2: ...ring the material in this document that conflict with these terms the warranty terms in the separate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license Restricted Rights Legend U S Government Restricted Rights Software and technical data rights ...

Page 3: ...ng Capillary Columns Consumables and Parts for Columns 30 To Install a Capillary Column Hanger 32 To Install Capillary Column Clips 33 To Condition a Capillary Column 34 To Cut a Loop from a Column 36 To Reverse a Column and Bakeout Contaminants 37 To Attach a Capillary Column Using UltiMetal Plus Flexible Metal Fittings 39 To Remove the Ferrule From a CFT Fitting 47 5 Maintaining the Split Splitl...

Page 4: ...Inlet 86 To Change the O Ring on the Purged Packed Inlet 87 To Change the Glass Liner on the Purged Packed Inlet 88 To Clean the Purged Packed Inlet 90 To Bakeout Contaminants from the Purged Packed Inlet 92 To Install a Packed Metal Column 93 To Install a Packed Column Adapter onto a Detector 95 To Install a Packed Glass Column 97 To Condition a Packed Column 99 To Install Ferrules on a Packed Me...

Page 5: ...et Consumables and Parts for the Programmable Temperature Vaporization Inlet 144 Exploded Parts View of the PTV Inlet 146 To Install a Capillary Column with the Programmable Temperature Vaporization Inlet 147 To Clean the Septumless Head on the PTV Inlet 150 To Replace the Septumless Head PTFE Ferrule on the PTV Inlet 152 To Change the Septum on the PTV Inlet 154 To Clean the Septum Seat in the Se...

Page 6: ...nal FID PTFE Chimney Insert 199 To Bakeout the FID 200 12 Maintaining the TCD Consumables and Parts for the Thermal Conductivity Detector 202 To Install a Capillary Column in the TCD 204 To Bakeout Contaminants from the TCD 207 13 Maintaining the NPD Consumables and Parts for the NPD 210 Exploded Parts View of the Nitrogen Phosphorus Detector 212 To Install a Capillary Column in the NPD 213 To Rep...

Page 7: ...ll the FPD Cover 253 Cleaning the FPD Brazement 254 16 Maintaining EPC Modules Consumables and Parts for the Aux EPC 256 Installing or Replacing Frits in the Aux EPC 258 Consumables and Parts for the PCM 260 Calibrating the PCM Interface 261 Installing or Replacing Frits in the PCM 262 17 Maintaining a Valve Consumables and Parts for Valves 266 Exploded Parts View of GC Rotary Valves 267 To Replac...

Page 8: ...8 Maintaining Your GC ...

Page 9: ...nance 11 Preparing for Maintenance 13 Viewing Status Data 14 Finding a Replacement Part Number 16 This section provides an overview of the maintenance procedures included in this document It also lists the tools needed for routine maintenance and the information needed to safely perform the various maintenance task ...

Page 10: ...nd a procedure Included in this manual are chapters on maintaining the following GC components Capillary Columns Split Splitless Inlet SSL Purged Packed Inlet PPI Cool On Column Inlet COC Multimode Inlet MMI Programmable Temperature Vaporization Inlet PTV Volatiles Interface VI Flame Ionization Detector FID Thermal Conductivity Detector TCD Electron Capture Detector ECD Nitrogen Phosphorus Detecto...

Page 11: ...ey wrench 8710 2411 Electronic flow meter s or bubble meter s capable of calibrated measurements at 1 10 and 100 mL min flow ranges Electronic leak detector Magnifying loupe 20X 430 1020 Metric ruler Bench vise for setting Swagelok fittings Razor or sharp knife Tweezers or thin needle nose pliers 8710 0007 8710 0004 Needle nose pliers ESD wrist strap for installing new components 9300 1408 Gloves ...

Page 12: ... Your GC Gloves clean lint free nylon for handling contamination sensitive parts large 8650 0030 small 8650 0029 Steel wool 0 or 00 grade for cleaning an inlet s septum seating surfaces Included with the GC ship kits Table 1 Tools and materials for GC maintenance Common tools Part number ...

Page 13: ...Maintenance Maintenance Mode Start Maintenance Follow the prompts To exit maintenance mode and restore the previous GC settings select Finished If you turned off the GC or changed other settings return to the Maintenance Mode screen as needed Note that the Maintenance Mode ends when the GC is turned off For automated maintenance procedures available through the GC the GC will make the instrument s...

Page 14: ...e very useful during maintenance For example Instrument status Readiness state running state Instrument status details Not ready modules error modules warnings Module status details Actual Setpoint pairs for each module quick On Off for certain modules firmware version and instrument IP address Add an item to the GC status listing as follows ...

Page 15: ...1 About Maintaining the GC Viewing Status Data Maintaining Your GC 15 Select the desired item from the drop down list then touch Add ...

Page 16: ...ent data system Parts Finder will be installed If you want to install the tool on another computer Parts Finder is included on the Agilent GC and GC MS User Manuals Tools DVD To find a consumable or replacement part using Parts Finder navigate to the part graphically based on the part s location in the GC Figure 1 Quickly navigate to replacement parts by clicking on images of GC components Part nu...

Page 17: ...Cover 19 To Remove the Electronics Cover 20 This section describes how to remove covers as needed for routine maintenance Only the covers listed in this chapter should be removed Removing other GC covers can compromise the safety features of the GC leading to personal injury or damage to the instrument ...

Page 18: ... GC and insert the left side first then gently snap in the right side onto the GC WARNING Be careful With the power switch on potentially dangerous voltages also exist All electronics boards in the instrument The internal wires and cables connected to these boards The wires for the oven heater The covers shield these parts as the parts may be hot enough to cause burns Never remove a cover unless t...

Page 19: ...emove the Pneumatics Cover The pneumatics cover protects the flow manifolds in the back top of the GC 1 Disconnect any vent tubing connected to the split and septum purge vents 2 Press the buttons located on each side of the pneumatics cover and lift up to remove it from the GC ...

Page 20: ...h to cause burns Never remove a cover unless the instrument is unplugged CAUTION Raising the electronics cover exposes the GC electronics Without FPD installed 1 Turn off the GC and unplug the power cord 2 Raise or remove the detector top cover 3 Loosen the captive screws on the right side cover slide the cover backwards then remove 4 Loosen the captive screw located on the left side of the electr...

Page 21: ...rew located on the left side of the electronics cover 5 Reach under the back of the electronics cover to release the clip holding it in place then raise the electronics cover and remove 6 Loosen the two thumbscrews in the tray below the PMT and remove the two screws in the back of the tray 7 Remove the tray from the electronics cover Loosen captive screws on right side cover Electronics cover GC f...

Page 22: ...2 Removing Covers To Remove the Electronics Cover 22 Maintaining Your GC ...

Page 23: ...Maintaining Your GC 23 3 Maintaining the GC Consumables and Parts for General GC Maintenance 24 Parts Identification 26 To Change the Hydrogen Sensor Calibration Gas Cylinder 27 ...

Page 24: ... 5021 7107 Copper tubing 1 8 inch od 50 ft 5180 4196 Gas regulators Regulator 2 stage brass body stainless steel diaphragms 125 psi max CGA350 hydrogen argon methane with 1 8 inch fitting For 1 4 inch tubing purchase a 1 4 inch adapter 5183 4642 Regulator 2 stage brass body stainless steel diaphragms 125 psi max CGA346 air with 1 8 inch fitting For 1 4 inch tubing purchase a 1 4 inch adapter 5183 ...

Page 25: ...ilter charcoal 1 pk CP17972 Gas Clean filter kit for TCD CP738408 Gas Clean Filter kit connecting unit for one filter including one carrier gas filter 1 8 inch connections a smart sensor and mounting bracket for the GC for carrier gas only CP179880 Gas Clean Filter kit connecting unit for four filters including four filters 1 4 inch connections for FID FPD NPD CP7995 Gas Clean Filter kit connectin...

Page 26: ...ntaining Your GC Parts Identification Figure 5 Hydrogen sensor calibration gas cylinder parts identification Pressure regulator Calibration gas cylinder Gas cylinder stand 1 8 inch Swagelok nut and ferrule 1 8 inch copper tubing cut to length needed ...

Page 27: ...ke sure the old cylinder is empty 2 Turn the pressure regulator completely off and set the output pressure as low as possible full CCW 3 Remove the pressure regulator from the old cylinder and install it onto the new cylinder 4 Install the new cylinder into the stand 5 Turn on the pressure in the new cylinder 6 Open the GC oven door and connect a flowmeter tube to the sensor tube in the oven 7 Sel...

Page 28: ...3 Maintaining the GC To Change the Hydrogen Sensor Calibration Gas Cylinder 28 Maintaining Your GC ...

Page 29: ...l a Capillary Column Hanger 32 To Install Capillary Column Clips 33 To Condition a Capillary Column 34 To Cut a Loop from a Column 36 To Reverse a Column and Bakeout Contaminants 37 To Attach a Capillary Column Using UltiMetal Plus Flexible Metal Fittings 39 To Remove the Ferrule From a CFT Fitting 47 ...

Page 30: ...o 320 mm columns Connect column to inlet or detector 5020 8292 250 Ferrule Vespel graphite 0 4 mm id 0 1 mm 0 2 mm and 0 25 mm capillary columns 5181 3323 10 pk Ferrule graphite 0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5080 8853 10 pk Column nut finger tight for 100 to 320 mm columns Connect column to inlet or detector 5020 8292 100 and 200 Ferrule Vespel graphite 0 37 mm id 0...

Page 31: ...apillary Columns Consumables and Parts for Columns Maintaining Your GC 31 Table 4 Capillary column hangers Description Part Number Column hanger 1460 1914 Capillary column clip kit for 7 inch column basket G1530 61580 ...

Page 32: ...t your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds 1 Place GC in maintenance mode Maintenance Instrument Perform Maintenance Maintenance Mode Start Maintenance Wait for the GC to become ready 2 Select either the front or back hanger position Hanger is shown in back position 3 I...

Page 33: ...ncture wounds 1 Gather the following Capillary column clip kit see Consumables and Parts for Columns on page 30 T 20 Torx screwdriver 2 Place GC in maintenance mode Maintenance Instrument Perform Maintenance Maintenance Mode Start Maintenance Wait for the GC to become ready 3 Loosen the four corner mounting screws but do not remove 4 Slip each corner screw through the large hole on the clip 5 Slid...

Page 34: ...ot enough to cause burns If the oven is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds 3 Install the column into the inlet using the new ferrules To Install a Capillary Column with the...

Page 35: ...gh to cause burns If the detector is hot wear gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds 10 Attach the column to the detector For details select your specific detector To Install a Capillary Column in the...

Page 36: ...ass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds 3 Loosen the inlet column nut and remove the column from the inlet 4 Uncoil one loop of column from the column hanger 5 Cut the unwanted loop from the column 6 Install the column into the inlet using the new ferrules To Install a Capillary Column with the Split Splitless Inlet To Install a Capillary...

Page 37: ...ition inlet and detector ends and place the column back on the hanger 6 Attach the column to the inlet To Install a Capillary Column with the Split Splitless Inlet To Install a Capillary Column with the Multimode Inlet To Install a Capillary Column with the Purged Packed Inlet To Install a Capillary Column with the Cool On Column Inlet To Install a Capillary Column with the Programmable Temperatur...

Page 38: ...the inlet temperature to 300 C or 25 C above the normal operating temperature 12 Set the column oven 25 C above the GC method final oven temperature to bake contaminants out of the inlet mostly through the split vent Do not exceed the column manufacturer s maximum temperature limit 13 Bakeout for 30 minutes ...

Page 39: ...ting This procedure is used to attach a capillary column to a splitter or switch or an Ultimate Union 1 Gather the following UltiMetal Plus Flexible Metal ferrules See Table 5 Swaging tool G3440 80227 Two 1 4 inch open end wrenches Column cutting tool 5181 8836 Internal nut G2855 20530 Lint free gloves 2 Check the column end It should be square and free of cracks If needed trim it 3 Pass the colum...

Page 40: ...thread of the corresponding fittings Unlike other ferrule designs a reliable leak free seal is best made by tightening the internal nut to a recommended number of degrees not by applying more force Applying excessive force will not provide a better seal Also compressing the flexible ferrule less minimizes damage to fittings To swage the ferrule to the column a Find your ferrule type in Table 6 and...

Page 41: ...15 to 20 degrees clockwise to assure the ferrule is properly swaged onto the column See Figure 10 Figure 10 Ferrule swaged to column and internal nut Table 6 Degrees to tighten the internal nut for proper swaging Ferrule part number Degrees to tighten internal nut G3188 27501 50 100 degrees G3188 27502 30 70 degrees G3188 27503 20 50 degrees G3188 27504 60 degrees G3188 27505 40 90 degrees G3188 2...

Page 42: ...t This procedure is used to attach a capillary column to a splitter or switch or an Ultimate Union 1 Gather the following UltiMetal Plus Flexible Metal ferrules See Table 5 Swaging tool G3440 80218 Two 1 4 inch open end wrenches Column cutting tool 5181 8836 Column nut Lint free gloves 2 Check the column end It should be square and free of cracks If needed trim it See Figure 12 Figure 12 3 Pass th...

Page 43: ...n nut ferrule and swaging tool 4 Loosely thread the column nut into the swaging tool until you start to feel resistance The column should still slide freely See Figure 14 Figure 14 Thread the column nut onto the swaging tool 5 Adjust the column position in the tool until the column end aligns with the correct dimension for the inlet See Figure 15 ...

Page 44: ... seal Also compressing the flexible ferrule less minimizes damage to fittings To swage the ferrule to the column a Find your ferrule type in Table 7 and note the range of degrees to tighten the column nut b Tighten the column nut clockwise to the lower end of your ferrule s range c Check if the ferrule is gripping the column If yes stop If not continue to tighten the column nut in small 5 to 15 de...

Page 45: ...column nut 7 Using the 1 4 inch open ended wrench turn the column nut an additional 15 to 20 degrees clockwise to assure the ferrule is properly swaged onto the column See Figure 17 Figure 17 Ferrule swaged to column and column nut 8 Using the 1 4 inch open ended wrench remove the column nut from the swaging tool and column ...

Page 46: ...gure 18 shows both an incorrect and correct swaging symmetry Figure 18 Incorrect and correct swaging symmetry If your column and ferrule appear like the incorrect example in Figure 18 above it is possible that your swaging wrench is defective or worn out Try swaging with a new wrench or new nut Incorrect Correct ...

Page 47: ...the internal nut If the ferrule does not release from the fitting do not try to pull the column free Insert a pointed object such as a thumb pin or a paper clip into the ferrule release hole as shown in Figure 19 and press firmly You will hear a click as the ferrule releases Figure 19 Release the ferrule Ultimate Union fitting shown Ferrule release holes ...

Page 48: ...4 Maintaining Capillary Columns To Remove the Ferrule From a CFT Fitting 48 Maintaining Your GC ...

Page 49: ...t 54 To Change the Septum on the Split Splitless Inlet 58 To Clean the Septum Seat in the Insert Assembly of the Split Splitless Inlet 60 To Change the Liner and O Ring on the Split Splitless Inlet 62 To Replace the Gold Seal on the Split Splitless Inlet 65 To Replace the Filter in the Split Vent Trap for the Split Splitless Inlet 67 To Clean the Split Splitless Inlet 69 To Bakeout Contaminants fr...

Page 50: ...per no glass wool 800 µL Yes 5181 3315 Splitless MS Certified single taper glass wool Yes 5188 6568 Splitless Direct inject 2 mm id quartz 250 µL No 18740 80220 Splitless Direct inject 2 mm id 250 µL Yes 5181 8818 Directinject Headspace or purge and trap 1 5 mm id 140 µL No 18740 80200 Direct column connect Single taper splitless 4 mm id Yes G1544 80730 Direct column connect Dual taper splitless 4...

Page 51: ...universal Connect column to inlet or detector 5181 8830 2 pk Column cutter ceramic wafer Cutting capillary columns 5181 8836 4 pk Pencil diamond tipped Cutting capillary columns 420 1000 Ferrule tool kit Ferrule installation 440 1000 Table 9 Nuts ferrules and hardware for capillary columns continued Column id mm Description Typical use Part number quantity Table 10 Other consumables and parts for ...

Page 52: ...52 Maintaining Your GC Column nut blanking plug 5020 8294 Capillary inlet preventative maintenance kit split 5188 6496 Capillary inlet preventative maintenance kit splitless 5188 6497 Table 10 Other consumables and parts for the split splitless inlet continued Description quantity Part number ...

Page 53: ...ploded Parts View of the Split Splitless Inlet Figure 20 Split splitless inlet exploded parts Column nut Ferrule Insulation cup Insulation Reducing nut Washer Inlet gold seal Retaining nut Septum Septum retainer nut Split splitless inlet body Liner Split vent line Insert assembly O ring Merlin Microseal Merlin cap ...

Page 54: ... Maintenance Maintenance Mode Start Maintenance Wait for the GC to become ready WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these colum...

Page 55: ...lumn end by supporting it against the column cutter opposite the scribe Inspect the end with a magnifying loupe to make certain there are no burrs or jagged edges 8 Wipe the column walls with a tissue dampened with isopropanol to remove fingerprints and dust 9 Position the column so it extends 4 to 6 mm above the end of the ferrule Slide the septum up the column to hold the column nut at this posi...

Page 56: ... the column nut Finger tighten the column nut until it begins to grip the column 12 Tighten the column nut an additional 1 4 to 1 2 turn with a wrench so that the column cannot be pulled from the fitting with gentle pressure 13 Plug in the new column s Smart ID key See Figure 21 Figure 21 Insert Smart ID key 14 Configure the new column 15 Condition the column per the manufacturer s recommendation ...

Page 57: ... After the column is installed at both inlet and detector establish a flow of carrier gas and purge as recommended by the column manufacturer 19 Restore the analytical method For FID or FPD immediately turn off the flame For NPD immediately turn off the bead 20 After the GC becomes ready wait 10 minutes then ignite the detector flame or bead WARNING Be careful The oven inlet and or detector may be...

Page 58: ... the septum those same steps are repeated below WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands 3 Remove the septum retainer nut or Merlin cap 4 Use tweezers to remove the septum or Merlin Microseal from the insert assembly Do not gouge or scratch the interior of the insert assembly 5 Firmly press the ne...

Page 59: ...ss Inlet Maintaining Your GC 59 7 Select Maintenance Inlets Septum injections then touch Reset Counter 8 Perform an inlet Leak Restriction test and reset the maintenance counters 9 Select Finished then select OK to exit the GC maintenance wizard 10 Restore the analytical method 1 mm ...

Page 60: ... C and wait for the inlet oven and other parts you might come into contact with inside the oven to cool before continuing Alternately place the GC in maintenance mode Maintenance Instrument Perform Maintenance Maintenance Mode Start Maintenance WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands 3 Slide the loc...

Page 61: ...he inlet body and push down to connect Slide the locking tab to the left 9 Firmly press the new septum or Merlin Microseal into the fitting See To Change the Septum on the Split Splitless Inlet on page 58 10 Replace the septum retainer nut or Merlin cap and finger tighten See To Change the Septum on the Split Splitless Inlet on page 58 11 On the GC touchscreen select Maintenance Inlets Septum inje...

Page 62: ...loves 2 Launch the GC maintenance wizard Maintenance Inlets select the inlet then select Perform Maintenance Replace Liner Start Maintenance The wizard will walk through the steps needed to replace the liner and O ring those same steps are repeated below WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands 3 Sli...

Page 63: ... Split Splitless Inlet Maintaining Your GC 63 5 Grasp the liner with tweezers and pull it out 6 Inspect the surface of the gold seal for graphite or rubber septum contamination If required replace the gold seal See To Replace the Gold Seal on the Split Splitless Inlet on page 65 ...

Page 64: ... liner contacts the gold seal 11 Line up the tab on the bottom of the insert assembly with the slot on the inlet body and push down to connect Slide the locking tab to the back 12 Turn on the inlet Allow the inlet and column to purge with carrier gas for 15 minutes before heating the inlet or the column oven 13 Bakeout contaminants See To Bakeout Contaminants from the Split Splitless Inlet on page...

Page 65: ...rm Maintenance Maintenance Mode Start Maintenance Wait for the GC to become ready WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands 3 Remove the inlet liner 4 Remove the column from the inlet Cap the open end of the column to prevent contamination Remove the insulation cup around the base of the inlet 5 Loose...

Page 66: ...educing nut and tighten securely with a wrench 8 Replace the inlet liner 9 Install the column and the insulation cup 10 Bakeout contaminants See To Bakeout Contaminants from the Split Splitless Inlet on page 71 11 Perform an inlet Leak Restriction test and reset the maintenance counters 12 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 13 Restore ...

Page 67: ...ted below WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands WARNING The split vent trap may contain residual amounts of any samples or other chemicals you have injected into the GC Follow your company s safety procedures for handling these types of substances while replacing the trap filter cartridge 3 Remove...

Page 68: ... filter cartridge then reassemble the trap using your fingers to fully tighten the knurled nut The nut should thread easily If the knurled nut does not thread easily loosen reassemble the 2 parts of the trap and thread again Do not force it 9 The GC maintenance wizard will perform checks at the appropriate times including Leak Restriction tests and will automatically reset the maintenance counters...

Page 69: ...aintenance Mode Start Maintenance WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands 3 Remove the inlet liner O ring and septum See To Change the Liner and O Ring on the Split Splitless Inlet on page 62 4 Disconnect the column from the inlet 5 Remove the reducing nut gold seal and washer See To Replace the ...

Page 70: ...t and reset the maintenance counters 14 Bakeout contaminants See To Bakeout Contaminants from the Split Splitless Inlet on page 71 15 On the GC touchscreen select Maintenance Inlets then touch Reset Counter 16 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 17 Restore the analytical method ...

Page 71: ...t the detector 25 C above normal operating temperature WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If they are hot wear heat resistant gloves to protect your hands 6 If the column is not attached to the detector cap the detector fitting 7 Set the inlet temperature to 300 C or 25 C above the normal operating temperature to bakeout contaminants from the inlet m...

Page 72: ...5 Maintaining the Split Splitless Inlet To Bakeout Contaminants from the Split Splitless Inlet 72 Maintaining Your GC ...

Page 73: ...um Seat in the Purged Packed Inlet 84 To Install an Adapter on the Purged Packed Inlet 86 To Change the O Ring on the Purged Packed Inlet 87 To Change the Glass Liner on the Purged Packed Inlet 88 To Clean the Purged Packed Inlet 90 To Bakeout Contaminants from the Purged Packed Inlet 92 To Install a Packed Metal Column 93 To Install a Packed Column Adapter onto a Detector 95 To Install a Packed G...

Page 74: ...263 50 pk 11 mm septum with partial through hole low bleed red 5181 3383 50 pk 11 mm septum low bleed gray 5080 8896 50 pk Merlin Microseal septum 30 psi 5181 8815 11 mm high temperature silicone septum 350 C and higher 5182 0739 50 pk Viton O ring Top insert weldment 5080 8898 12 pk Packed column adapters for detectors 1 8 inch Packed column adapter assembly G3435 81340 1 4 inch Packed column ada...

Page 75: ...0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5080 8853 10 pk Column nut finger tight for 100 to 320 mm columns Connect column to inlet or detector 5020 8292 250 Ferrule Vespel graphite 0 4 mm id 0 1 mm 0 2 mm and 0 25 mm capillary columns 5181 3323 10 pk Ferrule graphite 0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5080 8853 10 pk Column nut finger tight for 100 t...

Page 76: ...sumables and Parts for the Purged Packed Inlet 76 Maintaining Your GC Ferrule tool kit Ferrule installation 440 1000 Table 13 Nuts ferrules and hardware for capillary columns continued Column id mm Description Typical use Part number quantity ...

Page 77: ... Inlet Maintaining Your GC 77 Exploded Parts View of the Purged Packed Inlet Figure 24 Purged packed inlet exploded parts Column nut Ferrule Insulation cup Insulation Adapter Adapter nut Ferrule Glass liner O ring Top insert weldment Merlin Microseal Merlin cap Septum nut Septum ...

Page 78: ...e ready WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds 3 Install a 0 53 mm column adapter See ...

Page 79: ...inst the column cutter opposite the scribe Inspect the end with a magnifying loupe to make certain there are no burrs or jagged edges 8 Wipe the column walls with a tissue dampened with isopropanol to remove fingerprints and dust 9 Position the column so it extends 1 to 2 mm above the end of the ferrule Slide the septum up the column to hold the column nut at this fixed position 10 Thread the colu...

Page 80: ...ting with gentle pressure 13 Plug in the new column s Smart ID key See Figure 25 Figure 25 Insert Smart ID key 14 Configure the new column 15 Condition the column per the manufacturer s recommendation See To Condition a Capillary Column 16 Install the column into the detector To Install a Capillary Column in the FID To Install a Capillary Column in the NPD To Install a Capillary Column in the TCD ...

Page 81: ... turn off the flame For NPD immediately turn off the bead 20 After the GC becomes ready wait 10 minutes then ignite the detector flame or adjust offset on the NPD bead WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If the oven inlet or detector is hot wear heat resistant gloves to protect your hands 21 Allow the oven inlet and detector to equilibrate at operatin...

Page 82: ...aintenance The wizard will walk through the steps needed to replace the septum those same steps are repeated below WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands 3 Remove the septum retainer nut or Merlin cap 4 Use tweezers to remove the septum or Merlin Microseal from the retainer nut Do not gouge or s...

Page 83: ... mm above the nut CAUTION Overtightening the septum nut can cause contamination 7 On the GC touchscreen select Maintenance Inlets Septum injections then touch Reset Counter 8 The GC maintenance wizard will perform checks at the appropriate times including Leak Restriction tests and will automatically reset the maintenance counters 9 Select Finished then select OK to exit the GC maintenance wizard ...

Page 84: ...ands 3 Remove the septum retainer nut or Merlin cap 4 Loosen the top insert assembly and remove CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 5 Use tweezers to remove the septum or Merlin Microseal from the top insert assembly Do not gouge or scratch the interior of the septum head 6 Scrub the residue from the top insert assembly and septum nut with ...

Page 85: ...5 12 On the GC touchscreen select Maintenance Inlets Septum injections then select Reset Counter 13 Perform an inlet Leak Restriction test and reset the maintenance counters 14 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 15 Restore the analytical method 1 mm ...

Page 86: ...y WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 3 Clean the end of the adapter with a lint free cloth and methanol to remove contamination such as fingerprints 4 Place the tubing nut and Vespel graphite ferrul...

Page 87: ...and O ring those same steps are repeated below WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands 3 Loosen the top insert assembly to remove the top portion of the inlet CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 4 Use tweezers to remove the old O ring 5 In...

Page 88: ...The wizard will walk through the steps needed to replace the liner those same steps are repeated below WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands 3 Loosen the top insert assembly to remove the top portion of the inlet 4 Use a thin wire or wood splint to carefully lift and remove the old glass liner ...

Page 89: ...n is installed remove the column install the glass liner and replace the column See To Install a Capillary Column with the Purged Packed Inlet on page 78 7 Install the top insert assembly and hand tighten firmly 8 Configure the new liner 9 The GC maintenance wizard will perform checks at the appropriate times including Leak Restriction tests and will automatically reset the maintenance counters 10...

Page 90: ...enance WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands 3 Remove the column 4 Remove the septum nut and septum 5 Remove the top insert assembly 6 Remove the glass liner and O ring 7 If used remove the adapter 8 Ultrasonically clean the septum nut top insert assembly and adapter if used in a suitable solve...

Page 91: ...acked Inlet on page 82 16 Attach the column See To Install a Capillary Column with the Purged Packed Inlet on page 78 17 Set the septum and glass liner counters 18 Perform the inlet Leak Restriction test and reset the maintenance counters 19 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 20 Restore the analytical method ...

Page 92: ...etector 25 C above normal operating temperature If the column is not attached to the detector cap the detector fitting WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If they are hot wear heat resistant gloves to protect your hands 4 Set the inlet temperature to 300 C or 25 C above the normal operating temperature 5 Set the column oven 25 C above the GC method fi...

Page 93: ...th a wrench for a 1 8 inch column or an additional 3 4 turn for a 1 4 inch column Use two wrenches one on the column nut and the other on the adapter to prevent the adapter from rotating 7 Press Settings Configuration Columns then select Columns 1 through 6 Select Column Type Packed then choose your Inlet and Outlet Connection to identify the inlet and detector to which the column is attached 8 Sc...

Page 94: ...metal columns 17 Heat the oven to 200 C cool it to a safe handling temperature then re tighten the column connection Re tighten until snug only about 15 degrees rotation Repeat two more times This process will set the Vespel graphite ferrule to help prevent leaks 18 Restore the analytical method For FPD immediately turn off the flame For NPD immediately turn off the bead 19 After the GC becomes re...

Page 95: ...Mode Start Maintenance Wait for the GC to become ready WARNING Be careful The oven and or detector may be hot enough to cause burns If the detector is hot wear gloves to protect your hands CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils Handle the adapter carefully and install the packed column before installing the adapter into the detector base The t...

Page 96: ...ntenance Instrument Perform Maintenance Maintenance Mode Finished After installation heat the oven to 200 C cool it to a safe handling temperature then re tighten the column connection Re tighten until snug only about 15 degrees rotation Repeat two more times This process will set the Vespel graphite ferrule to help prevent leaks Detector ﬁtting ...

Page 97: ...errule on each end of the column Glass columns must be simultaneously inserted into the inlet and detector and installed parallel to the oven door When conditioning the column do not attach the column to the detector 4 If conditioning the column insert the column into the purged packed inlet until it bottoms Withdraw the column 1 to 2 mm Finger tighten the inlet column nut See To Condition a Packe...

Page 98: ...ntenance Instrument Perform Maintenance Maintenance Mode Finished 13 Establish a flow of carrier gas and purge as recommended by the packing manufacturer Generally 20 to 30 mL min for 2 mm id glass or 1 8 inch od metal columns 50 to 60 mL min for 4 mm id glass or 1 4 inch od metal columns 14 Restore the analytical method For FPD immediately turn off the flame For NPD immediately turn off the bead ...

Page 99: ...n page 93 4 If present remove the packed column adapter from the detector base If it is installed to the column it can be conditioned with the column 5 Cap the detector fitting with the no hole ferrule and column nut or with a blanking nut 6 Enter a column flow as recommended by the packing manufacturer or an appropriate flow as follows 20 to 30 mL min for 2 mm id glass or 1 8 inch od metal column...

Page 100: ...d deformation 3 Secure the fitting in a bench vise CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 4 Assemble a Swagelok nut and ferrules onto the column 5 Fully insert the column into the vise held fitting then withdraw 1 2 mm Finger tighten the nut 6 Tighten the nut an additional 3 4 turn with a wrench for a 1 8 inch column or an additional 1 1 4 tur...

Page 101: ... Cool On Column Inlet 106 To Check the Needle to Column Size on the COC Inlet 109 To Change a Septum on the COC Inlet 110 To Install an Insert on the COC Inlet 112 To Clean the COC Inlet 114 To Replace the 7693A Injector Needle Support Guide 116 To Replace a Needle in a Syringe 117 To Replace the Fused Silica Needle in a Syringe for the COC Inlet 118 To Bakeout Contaminants from the COC Inlet 119 ...

Page 102: ...45 60760 Needle support assembly 530 µm for 7683B injector G2913 60977 Table 15 Recommended parts for injections onto 0 53 mm aluminum clad columns Column type Part number Insert aluminum clad 0 53 mm id 19245 20780 4 rings Septum nut 530 µm G1545 80530 Syringe barrel removable needle 5 µL 5182 0836 Needle 530 µm 3 pk 5182 0832 Plunger button 10 pk for manual injections using syringe barrel 5182 0...

Page 103: ...quantity Insert fused silica 0 20 mm id 19245 20510 Cooling tower assembly 19320 80625 Syringe barrel for fused silica needle 10 µL 9301 0658 Replacement needles fused silica 0 18 mm 19091 63000 6 pk Replacement PTFE ferrule for fused silica syringe 0100 1389 Removable stainless steel needle syringe 10 µL 5182 9633 Replacement stainless steel needles 0 23 mm 5182 9645 3 pk On column insert spring ...

Page 104: ...t for 100 to 320 mm columns Connect column to inlet or detector 5020 8292 250 Ferrule Vespel graphite 0 4 mm id 0 1 mm 0 2 mm and 0 25 mm capillary columns 5181 3323 10 pk Ferrule graphite 0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5080 8853 10 pk Column nut finger tight for 100 to 320 mm columns Connect column to inlet or detector 5020 8292 100 and 200 Ferrule Vespel graphite 0...

Page 105: ...olumn Inlet Maintaining Your GC 105 Exploded Parts View of the Cool On Column Inlet Figure 26 Cool on column inlet exploded parts Septum nut 0 53 mm Septum nut 0 25 mm and 0 32 mm columns Septum Spring Insert Ferrule Column nut Cooling tower assembly Duckbill septum ...

Page 106: ...et may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin...

Page 107: ...olumn into the inlet until it bottoms You should feel spring tension as you push up on the column Do not withdraw the column 9 Insert the column nut into the inlet fitting and finger tighten WARNING To avoid bending the inlet always use two wrenches Use a 5 16 inch wrench to support the inlet while tightening the column nut with a 1 4 inch wrench 10 Tighten the column nut an additional 1 4 turn wi...

Page 108: ... mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 17 After the column is installed at both inlet and detector establish a flow of carrier gas and purge as recommended by the column manufacturer 18 Restore the analytical method For FPD immediately turn off the flame For NPD immediately turn off the bead 19 After the GC becomes ready wait 10 minutes then ignite the de...

Page 109: ...d replaced the needle with one of the correct size See Consumables and Parts for the Cool On Column Inlet on page 102 and To Replace a Needle in a Syringe on page 117 or To Replace the Fused Silica Needle in a Syringe for the COC Inlet on page 118 4 Identify the correct insert for the column size See Consumables and Parts for the Cool On Column Inlet on page 102 Use the insert that is the same siz...

Page 110: ...r is hot wear heat resistant gloves to protect your hands CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 3 Replace the septum If you are using a septum nut grasp the knurling and unscrew Remove the old septum with tweezers Use tweezers to install a new septum Push the septum into the septum nut until properly seated Firmly tighten the nut If you are u...

Page 111: ...e GC touchscreen select Maintenance Inlets Septum injections then touch Reset Counter 6 The GC maintenance wizard will perform checks at the appropriate times including Leak Restriction tests and will automatically reset the maintenance counters 7 Select Finished then select OK to exit the GC maintenance wizard 8 Restore the analytical method For manual 200 µm injections with fused silica needle ...

Page 112: ...lean lint free gloves to prevent contamination of parts with dirt and skin oils 3 Remove the column from the inlet 4 Locate the septum nut or cooling tower assembly at the top of the inlet and remove it If the septum remains in the septum nut do not remove it unless you want to change it If necessary replace the existing septum or duckbill with a new one See To Change a Septum on the COC Inlet on ...

Page 113: ...er the new insert straight into the inlet from the top The insert can be installed either end up 9 Install the spring on top of the insert 10 Install the septum and septum nut or duckbill septum and cooling tower assembly and finger tighten 11 Install the column See To Install a Capillary Column with the Cool On Column Inlet on page 106 12 Exit maintenance mode Select Maintenance Instrument Perfor...

Page 114: ...use burns If either is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 3 Remove the column ...

Page 115: ...er and methanol 9 Dry the spring and insert with compressed air or nitrogen 10 Install the insert See To Install an Insert on the COC Inlet on page 112 11 Install the column See To Install a Capillary Column with the Cool On Column Inlet on page 106 12 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished ...

Page 116: ...tion for complete details 1 Open the injector door 2 Remove the syringe 3 Slide the syringe carriage up to the top position 4 Completely remove the T 10 Torx screw from the support foot Be careful to not let the screw fall into the turret assembly 5 Slide off the support foot 6 Slide on the new support foot 7 Replace the T 10 Torx screw and tighten 8 Install the appropriate syringe 9 Close the inj...

Page 117: ...syringe barrel cap and remove the spring 3 Make sure that the needle has the PTFE disk as shown below If the syringe barrel does not have the PTFE disk use the instructions in the syringe box to wrap the needle 4 Check the new needle for a small wire inserted for shipment Remove the wire if present 5 Slide the spring and the cap over the needle 6 Insert the needle into the syringe barrel 7 Screw t...

Page 118: ...old needle 3 Hold the syringe vertically and insert the new fused silica needle so it is visible inside the syringe barrel If the needle cannot be inserted into the syringe barrel the PTFE ferrule may be blocked You may need to replace the ferrule 4 Push the plunger down until it bottoms The needle will be flush with the plunger end 5 Finger tighten the retaining nut Pull the needle gently to be s...

Page 119: ... column is attached to the detector set the detector 25 C above normal operating temperature If the column is not attached to the detector cap the detector fitting WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If they are hot wear heat resistant gloves to protect your hands 5 Set the column oven 25 C above the GC method final oven temperature to bake contaminan...

Page 120: ...7 Maintaining the COC Inlet To Bakeout Contaminants from the COC Inlet 120 Maintaining Your GC ...

Page 121: ...Nut Adapter 125 To Install a Capillary Column with the Multimode Inlet 126 To Change the Septum on the MMI 130 To Clean the Septum Seat in the Insert Assembly of the MMI 132 To Change the Liner and O Ring on the MMI 134 To Replace the Filter in the Split Vent Trap for the MMI 137 To Clean the Multimode Inlet 139 To Bakeout Contaminants from the MMI 141 ...

Page 122: ...1 5 mm id 140 µL No 18740 80200 Direct column connect Single taper splitless 4 mm id Yes G1544 80730 Direct column connect Dual taper splitless 4 mm id Yes G1544 80700 Table 22 Nuts ferrules and hardware for capillary columns Column id mm Description Typical use Part number quantity 530 Ferrule Vespel graphite 0 8 mm id 0 45 mm and 0 53 mm capillary columns 5062 3512 10 pk Ferrule graphite 1 0 mm ...

Page 123: ...y columns 420 1000 Ferrule tool kit Ferrule installation 440 1000 Table 22 Nuts ferrules and hardware for capillary columns continued Column id mm Description Typical use Part number quantity Table 23 Other consumables and parts for the multimode inlet MMI Description quantity Part number Septum retainer nut for headspace 18740 60830 Septum retainer nut 18740 60835 11 mm septum high temperature lo...

Page 124: ...ing Your GC Exploded Parts View of the MMI Figure 28 Multimode inlet exploded parts Septum retainer nut Septum Merlin cup Merlin Microseal O ring Liner Split vent line Insulation Insulation cup Column nut Screws Inlet base Split vent line Cryo for CO2 Insert assembly ...

Page 125: ...intenance Instrument Perform Maintenance Maintenance Mode Start Maintenance Wait for the GC to become ready WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands 3 When the GC is ready open the GC oven door 4 Thread the column adapter nut onto the base of the inlet The nut must spin freely before it can be used t...

Page 126: ...intenance Mode Start Maintenance Wait for the GC to become ready WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent p...

Page 127: ...supporting it against the column cutter opposite the scribe Inspect the end with a magnifying loupe to make certain there are no burrs or jagged edges 8 Wipe the column walls with a tissue dampened with isopropanol to remove fingerprints and dust 9 Position the column so it extends 10 to 12 mm above the end of the ferrule Slide the septum up the column to hold the column nut at this position Ferru...

Page 128: ...just the column position so that the septum contacts the bottom of the column nut Finger tighten the column nut until it begins to grip the column 12 While holding the inlet base with one wrench use the second wrench to tighten the column nut an additional 1 4 to 1 2 turn so that the column cannot be pulled from the fitting with gentle pressure 13 Plug in the new column s Smart ID key See Figure 2...

Page 129: ... Instrument Perform Maintenance Maintenance Mode Finished 18 After the column is installed at both inlet and detector establish a flow of carrier gas and purge as recommended by the column manufacturer 19 Restore the analytical method For FID or FPD immediately turn off the flame For NPD immediately turn off the bead 20 After the GC becomes ready wait 10 minutes then ignite the detector flame or b...

Page 130: ...d below WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands 3 Remove the septum retainer nut or Merlin cap 4 Use tweezers to remove the septum or Merlin Microseal from the insert assembly Do not gouge or scratch the interior of the insert assembly 5 Firmly press the new septum or Merlin Microseal into the fi...

Page 131: ...nce Inlets Septum injections then touch Reset Counter 8 The GC maintenance wizard will perform checks at the appropriate times including Leak Restriction tests and will automatically reset the maintenance counters 9 Select Finished then select OK to exit the GC maintenance wizard 10 Restore the analytical method 1 mm ...

Page 132: ...e continuing Alternately place the GC in maintenance mode Maintenance Instrument Perform Maintenance Maintenance Mode Start Maintenance WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands 3 Slide the locking tab forward counterclockwise Lift the insert assembly straight up and away from the inlet to avoid chipp...

Page 133: ... Firmly press the new septum or Merlin Microseal into the fitting See To Change the Septum on the MMI on page 130 10 Replace the septum retainer nut or Merlin cap and finger tighten See To Change the Septum on the MMI on page 130 11 Perform an inlet Leak Restriction test and reset the maintenance counters 12 On the GC touchscreen select Maintenance Inlets Septum injections then select Reset Counte...

Page 134: ...wizard Maintenance Inlets select the multimode inlet then select Perform Maintenance Replace Liner Start Maintenance The wizard will walk through the steps needed to replace the liner and O ring those same steps are repeated below WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands 3 Slide the locking tab forwa...

Page 135: ...ng the MMI To Change the Liner and O Ring on the MMI Maintaining Your GC 135 5 Grasp the liner with tweezers and pull it out 6 Inspect the surface of the seal for contamination If required clean with cotton swabs ...

Page 136: ... the liner contacts the seal 9 Line up the tab on the bottom of the insert assembly with the slot on the inlet body and push down to connect Slide the locking tab to the back 10 Turn on the inlet Allow the inlet and column to purge with carrier gas for 15 minutes before heating the inlet or the column oven 11 Bakeout contaminants See To Bakeout Contaminants from the MMI on page 141 12 The GC maint...

Page 137: ...ARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands WARNING The split vent trap may contain residual amounts of any samples or other chemicals you have injected into the GC Follow your company s safety procedures for handling these types of substances while replacing the trap filter cartridge 3 Remove the To Rem...

Page 138: ... then reassemble the trap using your fingers to fully tighten the knurled nut The nut should thread easily If the knurled nut does not thread easily loosen reassemble the 2 parts of the trap and thread again Do not force it 9 The GC maintenance wizard will perform checks at the appropriate times including Leak Restriction tests and will automatically reset the maintenance counters 10 Install the p...

Page 139: ...to cool before continuing Alternately place the GC in maintenance mode Maintenance Instrument Perform Maintenance Maintenance Mode Start Maintenance WARNING Be careful The oven and or inlet may be hot enough to cause burns If the inlet is hot wear heat resistant gloves to protect your hands 3 Turn off the GC CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin o...

Page 140: ...s 3 5 if necessary to remove any remaining deposits 10 Using clean solvent rinse the inlet volume several times but never overfill the inlet bore Position a container under the column opening in the inlet to catch the used solvent exiting the bottom of the MMI 11 Allow the inlet to dry 12 Install the liner and O ring 13 Reinstall the column 14 Turn on the GC 15 Perform an inlet Leak Restriction te...

Page 141: ...ormal operating temperature WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If they are hot wear heat resistant gloves to protect your hands 6 If the column is not attached to the detector cap the detector fitting 7 Set the inlet temperature to 300 C or 25 C above the normal operating temperature to bakeout contaminants from the inlet mostly through the split ven...

Page 142: ...8 Maintaining the MMI To Bakeout Contaminants from the MMI 142 Maintaining Your GC ...

Page 143: ...n Inlet 147 To Clean the Septumless Head on the PTV Inlet 150 To Replace the Septumless Head PTFE Ferrule on the PTV Inlet 152 To Change the Septum on the PTV Inlet 154 To Clean the Septum Seat in the Septum Head Assembly of the PTV Inlet 155 To Change the Liner on the PTV Inlet 156 To Replace the Inlet Adapter for the PTV Inlet 158 To Replace the Filter in the Split Vent Trap for the PTV Inlet 16...

Page 144: ...les G2617 80540 Table 25 Other consumables and parts for the PTV inlet Description Part number Syringe 5 µL 23 gauge fixed needle 9301 0892 Syringe 10 µL 23 gauge fixed needle 9301 0713 Syringe 50 µL 23 gauge fixed needle for large volume injections 5183 0318 Syringe 100 µL 23 gauge fixed needle for large volume injections 5183 2058 Split vent trap PM kit single cartridge 5188 6495 Septumless head...

Page 145: ... 2M inlet 0 20 mm id 5182 9756 10 pk Ferrules for Graphpak 2M inlet 0 25 mm id 5182 9768 10 pk Ferrules for Graphpak 2M inlet 0 32 mm id 5182 9769 10 pk Ferrules for Graphpak 2M inlet 0 53 mm id 5182 9770 10 pk Split nut for Graphpak adapter 5062 3525 Includes 1 adapter 1 silver seal and 1 split column nut Table 25 Other consumables and parts for the PTV inlet continued Description Part number ...

Page 146: ...ature vaporization inlet exploded parts Septum nut Septum Septum head Septumless head assembly Kalrez seal Merlin cap Merlin Microseal Guide cap Valve body Pressure spring Viton seal Sealing element PTFE ferrule Graphpak 3D ferrule Liner PTV inlet assembly Silver seal Graphpak inlet adapter Ferrule for Graphpak adapter Column nut Carrier gas tube Ferrule ...

Page 147: ... WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds 3 Before installing the column install the correc...

Page 148: ...l to remove fingerprints and dust 9 Position the column so it extends 17 mm above the end of the ferrule Mark the column behind the ferrule with typewriter correction fluid or a marker Slide the nut over the column 10 Insert the column into the adapter and finger tighten the column nut Looking through the slot in the nut adjust the column until the mark is correctly positioned below the Graphpak 2...

Page 149: ...ntenance Instrument Perform Maintenance Maintenance Mode Finished 17 After the column is installed at both inlet and detector establish a flow of carrier gas and purge as recommended by the column manufacturer 18 Restore the analytical method For FPD immediately turn off the flame For NPD immediately turn off the bead 19 After the GC becomes ready wait 10 minutes then ignite the detector flame or ...

Page 150: ...temperature to 40 C and wait for the inlet oven and other parts you might come into contact with inside the oven to cool before continuing Alternately place the GC in maintenance mode Maintenance Instrument Perform Maintenance Maintenance Mode Start Maintenance 3 Disconnect the carrier gas line WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat res...

Page 151: ...rrule on the PTV Inlet on page 152 12 Wearing clean lint free gloves reassemble the head in reverse order Be sure that the seals and the pressure spring are not damaged 13 Finger tighten the septumless head then tighten an additional 1 8 turn with a wrench 14 Reconnect the carrier gas line 15 Check for leaks if necessary slightly tighten the guide cap with the syringe needle inserted If the head l...

Page 152: ...inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands 3 Unscrew the guide cap from the septumless head and remove the PTFE ferrule 4 Push the guide cap and replacement ferrule over the syringe needle so that at least 10 mm of the needle tip is exposed 5 Guide the end of the needle into the septumless head until the ferrule meets the septumless hea...

Page 153: ...ntaining Your GC 153 12 Observe the inlet Total Flow Tighten the guide cap until the Total Flow stops decreasing typically near 8 mL min 13 Remove the syringe from the inlet and press 14 Restore the analytical method 15 Perform an inlet Leak Restriction test and reset the maintenance counters ...

Page 154: ... Merlin cap If the septum head begins to turn during removal support it manually while removing the cap 4 Use tweezers to remove the septum or Merlin Microseal from the retainer nut Do not gouge or scratch the interior of the septum head 5 Firmly press the new septum or Merlin Microseal into the fitting The metal parts side of the Merlin Microseal should face down toward the oven 6 Replace the sep...

Page 155: ... retainer nut or Merlin cap If the septum head begins to turn during removal support it manually while removing the cap 4 Unscrew the septum head assembly from the inlet and move it up and away from the inlet 5 Use tweezers to remove the septum or Merlin Microseal from the retainer nut Do not gouge or scratch the interior of the septum head 6 Scrub the residue from the retainer nut and septum hold...

Page 156: ...ed to replace the liner those same steps are repeated below WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 3 Remove the head from the inlet For septumless head disconnect the carrier gas line and unscrew and remov...

Page 157: ...ite within the ferrule is flush with the top of the metal collar 11 Insert the glass liner into the inlet from above until the unpacked side of the ferrule rests on the top of the inlet 12 Replace the head For septumless head screw the head onto the inlet and tighten 1 8 turn past finger tight with a wrench Reconnect the carrier gas line For septum head align the head with the inlet and manually e...

Page 158: ...m wrench Lint free gloves 3 Place GC in maintenance mode Maintenance Instrument Perform Maintenance Maintenance Mode Start Maintenance Wait for the GC to become ready WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils...

Page 159: ...rtightening will damage the inlet 7 Install the column See To Install a Capillary Column with the Programmable Temperature Vaporization Inlet on page 147 8 Check the adapter for leaks 9 Reset the silver seal EMF counter 10 Perform an inlet Leak Restriction test and reset the maintenance counters 11 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 12...

Page 160: ...are repeated below WARNING Be careful The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands WARNING The split vent trap may contain residual amounts of any samples or other chemicals you have injected into the GC Follow your company s safety procedures for handling these types of substances while replacing the trap filter cartridge...

Page 161: ...tridge then reassemble the trap using your fingers to fully tighten the knurled nut The nut should thread easily If the knurled nut does not thread easily loosen reassemble the 2 parts of the trap and thread again Do not force it 9 The GC maintenance wizard will perform checks at the appropriate times including Leak Restriction tests and will automatically reset the maintenance counters 10 Install...

Page 162: ...C above normal operating temperature WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If they are hot wear heat resistant gloves to protect your hands 6 If the column is not attached to the detector cap the detector fitting 7 Set the inlet temperature to 300 C or 25 C above the normal operating temperature to bakeout contaminants from the inlet mostly through the ...

Page 163: ...ace 164 Exploded Parts View of the VI 166 To Install a Capillary Column with the Volatiles Interface 167 To Remove the VI Interface 171 To Clean the VI 173 To Install the VI Interface 174 To Replace the Filter in the Split Vent Trap for the VI 175 To Bakeout Contaminants from the VI Inlet 177 ...

Page 164: ...hite 0 8 mm id 0 53 mm capillary columns 500 2118 10 pk Column nut finger tight for 0 53 mm columns Connect column to inlet or detector 5020 8293 320 Ferrule Vespel graphite 0 5 mm id 0 32 mm capillary columns 5062 3514 10 pk Ferrule graphite 0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5080 8853 10 pk Column nut finger tight for 100 to 320 mm columns Connect column to inlet or de...

Page 165: ...y ferrule 5020 8294 Column nut universal Connect column to inlet or detector 5181 8830 2 pk Column cutter ceramic wafer Cutting capillary columns 5181 8836 4 pk Pencil diamond tipped Cutting capillary columns 420 1000 Ferrule tool kit Ferrule installation 440 1000 Table 28 Nuts ferrules and hardware for capillary columns continued Column id mm Description Typical use Part number quantity ...

Page 166: ...g the VI Exploded Parts View of the VI 166 Maintaining Your GC Exploded Parts View of the VI Figure 36 Volatiles interface exploded parts Clamping plate Volatiles interface Ferrule column Column nut long Nut Ferrule ...

Page 167: ...resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 3 Place the column on the hanger with the ends pointing u...

Page 168: ...porting it against the column cutter opposite the scribe Inspect the end with a magnifying loupe to make certain that there are no burrs or jagged edges 7 Wipe the column walls with a tissue dampened with isopropanol to remove fingerprints and dust 8 Position the column so it extends 6 mm above the end of the ferrule Slide the septum up the column to hold the column nut at this fixed position Ferr...

Page 169: ...ector establish a flow of carrier gas through the transfer line Purge as recommended by the column manufacturer 15 Condition the column per the manufacturer s recommendation See To Condition a Capillary Column 16 Install the column into the detector To Install a Capillary Column in the FID To Install a Capillary Column in the NPD To Install a Capillary Column in the TCD To Install a Capillary Colu...

Page 170: ...fset on the NPD bead WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If the oven inlet or detector is hot wear heat resistant gloves to protect your hands 21 Allow the oven inlet and detector to equilibrate at operating temperature then retighten the fittings 22 Reset the EMF counter 23 Perform an inlet Leak Restriction test and reset the maintenance counters ...

Page 171: ... Start Maintenance Wait for the GC to become ready WARNING Be careful The interface may be hot enough to cause burns If the interface is hot wear gloves to protect your hands 3 Remove the column 4 Remove the transfer line by loosening the nut then lift it from the interface 5 Loosen the five inlet cover screws and remove the inlet cover 6 Remove the clamping plate from the interface by loosening t...

Page 172: ...10 Maintaining the VI To Remove the VI Interface 172 Maintaining Your GC 8 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished ...

Page 173: ...ough to cause burns If either is hot wear heat resistant gloves to protect your hands WARNING The split vent trap and line may contain residual amounts of any samples or other chemicals you have injected into the GC Follow your company s safety procedures for handling these types of substances 4 Remove the split vent and pressure sensing lines by loosening the nuts CAUTION Wear clean lint free glo...

Page 174: ... sensing lines and finger tighten the nuts Tighten an additional 1 4 turn with a wrench 3 Place the interface into the heater block and reseat the tubing as needed 4 Install the clamping plate and tighten the screw 5 Install the inlet cover Be sure the cover does not damage any tubing 6 Attach the sample transfer line 7 Install the column See To Install a Capillary Column with the Volatiles Interf...

Page 175: ...ul The oven and or inlet may be hot enough to cause burns If either is hot wear heat resistant gloves to protect your hands WARNING The split vent trap may contain residual amounts of any samples or other chemicals you have injected into the GC Follow your company s safety procedures for handling these types of substances while replacing the trap filter cartridge 3 Remove the pneumatics cover top ...

Page 176: ...then reassemble the trap using your fingers to fully tighten the knurled nut The nut should thread easily If the knurled nut does not thread easily loosen reassemble the 2 parts of the trap and thread again Do not force it 9 The GC maintenance wizard will perform checks at the appropriate times including Leak Restriction tests and will automatically reset the maintenance counters 10 Install the pn...

Page 177: ... normal operating temperature If the column is not attached to the detector cap the detector fitting WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If they are hot wear heat resistant gloves to protect your hands 6 Set the inlet and oven temperature to 300 C or 25 C above the normal operating temperature to bakeout contaminants from the inlet mostly through the ...

Page 178: ...10 Maintaining the VI To Bakeout Contaminants from the VI Inlet 178 Maintaining Your GC ...

Page 179: ... of the Flame Ionization Detector 182 To Install a Capillary Column in the FID 184 To Replace an FID Jet 187 To Perform Maintenance on the FID Collector Assembly 190 To Check the FID Leakage Current 197 To Check the FID Baseline 198 To Install the Optional FID PTFE Chimney Insert 199 To Bakeout the FID 200 ...

Page 180: ...0 mm columns Connect column to inlet or detector 5020 8292 250 Ferrule Vespel graphite 0 4 mm id 0 1 mm 0 2 mm and 0 25 mm capillary columns 5181 3323 10 pk Ferrule graphite 0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5080 8853 10 pk Column nut finger tight for 100 to 320 mm columns Connect column to inlet or detector 5020 8292 100 and 200 Ferrule Vespel graphite 0 37 mm id 0 1 m...

Page 181: ...0 Jet FID 0 011 inch id G4591 20320 Table 31 FID collector assembly parts Description Part number quantity Screw M4 25 mm Torx T20 0515 2712 3 pk Collector assembly G4591 60691 Collector nut 19231 20940 Spring washer 3050 1246 Ignitor castle 19231 20910 Ignitor castle Hastelloy 19231 21060 Upper lower collector insulator G1531 20700 Collector body G1531 20690 Collector body Hastelloy G1531 21090 S...

Page 182: ...182 Maintaining Your GC Exploded Parts Views of the Flame Ionization Detector Figure 40 Flame ionization detector FID assembly exploded parts PTFE chimney 25 mm screws Collector assembly Gasket Jet Spring FID interconnect Mounting pallet Ferrule Column adapter Ferrule Column nut ...

Page 183: ... collector assembly exploded parts view 25 mm screws Collector assembly Gasket Jet 25 mm screws Collector assembly Collector nut Spring washer Ignitor castle Upper collector insulator Collector body Spanner nut collector Collector mount Lower collector insulator Collector housing Gasket Ignitor glow plug assembly with O ring Ignitor cable assembly ...

Page 184: ...Be careful The oven inlet and or detector may be hot enough to cause burns If the oven inlet or detector is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds CAUTION Wear clean lint free ...

Page 185: ...ain there are no burrs or jagged edges 6 Wipe the column walls with a tissue dampened with isopropanol to remove fingerprints and dust 7 Install the capillary column If the column id is greater than 0 1 mm a Gently insert the column into the detector until it bottoms do not attempt to force it further b Finger tighten the column nut then withdraw the column about 2 mm Tighten the nut an additional...

Page 186: ...at this fixed position c Insert the column into the detector Slide the nut and ferrule up the column to the detector base Finger tighten the column nut until it grips the column d Adjust the column not the septum position so that the septum is even with the bottom of the column nut Tighten the nut an additional 1 4 turn with a wrench 8 Exit maintenance mode Select Maintenance Instrument Perform Ma...

Page 187: ... walk through the steps needed to replace the jet those same steps are repeated below WARNING Be careful The oven and or detector may be hot enough to cause burns If the detector is hot wear gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these colum...

Page 188: ... using solvent a swab and compressed air or nitrogen 8 Use tweezers to lower the new jet into the housing CAUTION Do not overtighten the jet Overtightening may permanently deform and damage the jet the detector base or both The torque specification is 10 inch pounds 9 Carefully screw the jet into the housing Tighten 1 6 turn past finger tight 1 6 turn is one flat on a typical screwdriver handle or...

Page 189: ...establish a flow of carrier gas and purge as recommended by the column manufacturer c Check the FID leakage current See To Check the FID Leakage Current on page 197 d Bakeout the detector See To Bakeout the FID on page 200 e Restore the analytical method WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If the oven inlet or detector is hot wear heat resistant glove...

Page 190: ...asket T 20 Torx screwdriver 1 4 inch nut driver Tweezers 5 16 inch wrench Lint free gloves Clean cloth CAUTION To avoid contaminating the FID wear clean lint free gloves when handling the collector assembly 2 Place GC in maintenance mode Maintenance Instrument Perform Maintenance Maintenance Mode Start Maintenance Wait for the GC to become ready WARNING Be careful The oven and or detector may be h...

Page 191: ...ssembly with copper washer skip to step 16 for assembly 5 Remove the three screws that secure the collector assembly to the FID mounting pallet CAUTION This step exposes the interconnect spring Be careful not to touch or disfigure the spring while working on the FID Any dirt or bending will reduce the sensitivity of your detector 6 Remove the collector assembly Place it on a clean cloth for additi...

Page 192: ... Lift the castle out of the collector housing When removing the castle some of the collector parts may be attached Set these on a clean cloth to protect from scratches or dirt 9 If only replacing the FID castle skip to step 15 for reassembly 10 Remove the collector and insulators a If needed remove the collector and upper insulator from the FID housing The lower insulator may come out with the col...

Page 193: ...nd place the parts on a clean cloth 11 Remove the collector housing from the mount if necessary 12 Use tweezers to remove the gasket from the bottom of the housing The collector assembly is now completely disassembled Reassemble as follows 13 Use tweezers to install a new gasket onto the housing being sure that it lays flat on the brass surface ...

Page 194: ... the housing Seat the insulator with the flat surface facing out of the housing b Insert the long end of collector into the housing and lower insulator c Insert the other insulator onto the top of the collector with the flat surface facing towards the housing 15 Install the FID ignitor castle a Orient the castle so that the threaded hole for the ignitor faces toward the electronics ...

Page 195: ...Install the collector nut over the castle and tighten firmly The seal should be airtight Maintain the orientation of the ignitor hole with the base as shown below 16 Install the FID ignitor a Insert the ignitor and copper seal into the threaded hole of the castle Keep the mating threads clean b Tighten the ignitor with a wrench Ignition requires a good electrical contact that is free of any dirt ...

Page 196: ...h pounds 19 Connect the ignitor extension cable 20 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 21 Verify assembly a Check the FID leakage current See To Check the FID Leakage Current on page 197 b Bakeout the detector See To Bakeout the FID on page 200 c Check the FID baseline See To Check the FID Baseline on page 198 22 Reset the EMF counters ...

Page 197: ...eakage Current Tests Read the Test Details screen then press Start Test 3 Turn off the FID flame 4 Show the detector output signal in Status On the GC touchscreen go to Home Status listing Add Select Detector s Output from the drop down list then touch Add 5 Verify that the output is stable and 1 0 pA If the output is unstable or 1 0 pA turn off the GC and check for proper assembly of the upper FI...

Page 198: ... output signal in Status On the GC touchscreen go to Home Status listing Add Select Detector s Output from the drop down list then touch Add 4 When the flame is lit and the GC is ready verify that the output is stable and 20 pA If the output is not stable or 20 pA the system or gas may be contaminated If this contamination is isolated to the detector then bakeout the FID See To Bakeout the FID on ...

Page 199: ...l the Optional FID PTFE Chimney Insert WARNING Be careful The detector may be hot enough to cause burns If the detector is hot wear heat resistant gloves to protect your hands 1 Light the FID flame 2 Insert the PTFE chimney into the FID castle NOTE When installed the PTFE chimney insert prevents ignition ...

Page 200: ...vent an oven explosion 3 Maintain inert carrier gas flow through the column or remove the column from the GC 4 Set the detector temperature at 350 to 375 C 5 Set normal operating flows 6 Light the FID flame 7 Set the oven temperature to 250 C or 25 C above the normal maximum operating temperature Do not exceed the column s temperature limit 8 Hold at temperature for 30 minutes or until the baselin...

Page 201: ...Maintaining Your GC 201 12 Maintaining the TCD Consumables and Parts for the Thermal Conductivity Detector 202 To Install a Capillary Column in the TCD 204 To Bakeout Contaminants from the TCD 207 ...

Page 202: ... pk Column nut finger tight for 100 to 320 mm columns Connect column to inlet or detector 5020 8292 250 Ferrule Vespel graphite 0 4 mm id 0 1 mm 0 2 mm and 0 25 mm capillary columns 5181 3323 10 pk Ferrule graphite 0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5080 8853 10 pk Column nut finger tight for 100 to 320 mm columns Connect column to inlet or detector 5020 8292 100 and 200...

Page 203: ...D Standard TCD column hardware Maintaining Your GC 203 Table 33 Packed column adapters Description Part number quantity 1 8 inch Packed column adapter assembly G3435 81340 1 4 inch Packed column adapter assembly G3435 81330 ...

Page 204: ...eady WARNING Be careful The oven inlet and or detector may be hot enough to cause burns If the oven inlet or detector is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds CAUTION Wear cle...

Page 205: ...ain there are no burrs or jagged edges 6 Wipe the column walls with a tissue dampened with isopropanol to remove fingerprints and dust 7 Install the capillary column If the column id is greater than 0 1 mm a Gently insert the column into the detector until it bottoms do not attempt to force it further b Finger tighten the column nut then withdraw the column about 2 mm Tighten the nut an additional...

Page 206: ...ndferruleatthis fixed position c Insert the column into the detector Slide the nut and ferrule up the column to the detector base Finger tighten the column nut until it grips the column d Adjust the column not the septum position so that the septum is even with the bottom of the column nut Tighten the nut an additional 1 4 turn with a wrench 8 Exit maintenance mode Select Maintenance Instrument Pe...

Page 207: ...at resistant gloves to protect your hands 2 Turn off the TCD filament 3 If the column is attached to the inlet maintain inert carrier gas flow through the column WARNING If using hydrogen as a carrier gas turn off the hydrogen supply and cap the end of the column to prevent an oven explosion 4 Set the reference gas flow rate between 20 and 30 mL min 5 Set the detector temperature to 375 C 6 Hold a...

Page 208: ...12 Maintaining the TCD To Bakeout Contaminants from the TCD 208 Maintaining Your GC ...

Page 209: ...the NPD 210 Exploded Parts View of the Nitrogen Phosphorus Detector 212 To Install a Capillary Column in the NPD 213 To Replace the NPD Bead Assembly 216 To Maintain the NPD Collector Ceramic Insulators and Jet 220 To Check the NPD Leakage Current 225 To Bakeout the NPD 226 ...

Page 210: ...pk Ferrule Vespel graphite 1 8 inch for packed column adapters 0100 1332 10 pk Nut 1 4 inch brass for packed column adapters 5180 4105 10 pk Ferrule Vespel 1 4 inch for packed column adapters 5080 8774 10 pk 1 8 inch Packed column adapter assembly G3435 81340 1 4 inch Packed column adapter assembly G3435 81330 Table 35 Nuts ferrules and hardware for capillary columns Column id mm Description Typic...

Page 211: ...columns 5181 3323 10 pk Ferrule graphite 0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5080 8853 10 pk Ferrule graphite 0 4 mm id 500 2114 10 pk Column nut finger tight for 100 to 320 mm columns Connect column to inlet or detector 5020 8292 All Ferrule no hole Testing 5181 3308 10 pk Capillary column blanking nut Testing use with any ferrule 5020 8294 Column nut universal Connect c...

Page 212: ...ded Parts View of the Nitrogen Phosphorus Detector Figure 43 Nitrogen Phosphorus Detector NPD exploded parts NPD cover Screws Bead assembly Screws Lid Metal C ring top Ceramic insulator upper Collector Metal C ring bottom Ceramic insulator lower Metal C ring bottom Jet Electrometer Column nut Insulation cover ...

Page 213: ...Be careful The oven inlet and or detector may be hot enough to cause burns If the oven inlet or detector is hot wear heat resistant gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds CAUTION Wear clean lint free ...

Page 214: ...ain there are no burrs or jagged edges 6 Wipe the column walls with a tissue dampened with isopropanol to remove fingerprints and dust 7 Install the capillary column If the column id is greater than 0 1 mm a Gently insert the column into the detector until it bottoms do not attempt to force it further b Finger tighten the column nut then withdraw the column about 2 mm Tighten the nut an additional...

Page 215: ...ndferruleatthis fixed position c Insert the column into the detector Slide the nut and ferrule up the column to the detector base Finger tighten the column nut until it grips the column d Adjust the column not the septum position so that the septum is even with the bottom of the column nut Tighten the nut an additional 1 4 turn with a wrench 8 Exit maintenance mode Select Maintenance Instrument Pe...

Page 216: ...id touching the bead with your fingers and prevent it from coming in contact with other surfaces 4 Turn off the NPD bead and enable the Dry Bead and Auto Adjust settings Agilent data system users After turning off the bead save the data system method and shut down the instrument session Note that in some data system versions you may need to use the GC touchscreen for these settings To do this the ...

Page 217: ...e the NPD Bead Assembly Maintaining Your GC 217 Figure 44 Remove NPD cover 9 Twist the ring to disconnect the bead assembly cable Push and twist the lock so that the button slides up in the groove then pull the cable ends apart 1 2 3 ...

Page 218: ...vering the new bead 13 Mount the new bead assembly on the NPD lid Be careful not to bump the bead on the sides of the lid or collector 14 Replace the screws Finger tighten the first screw tighten the remaining screws normally and then completely tighten the first screw Do not overtighten the screws 15 Carefully bend the bead assembly so it will mate with the bead power cable 16 Reconnect the bead ...

Page 219: ...old for 15 minutes 21 Increase the temperature to operating value 310 to 320 C recommended Allow 15 minutes for equilibration 22 Check the NPD leakage current See To Check the NPD Leakage Current on page 225 If 2 0 pA verify bead installation or see the Troubleshooting manual 23 If using an Agilent data system connect to the instrument 24 Restore the analytical method Confirm the detector hydrogen...

Page 220: ...lation 1 Gather the following NPD ceramic insulator kit see Consumables and Parts for the NPD on page 210 Collector Cap for the bead T 10 and T 20 Torx screwdrivers Tweezers Cotton swab Solvent Methanol Jet Lint free gloves Compressed filtered dry air or nitrogen CAUTION The bead is delicate Be careful not to break or crack the bead When performing maintenance on the NPD avoid touching the bead wi...

Page 221: ...ing on the FID Any dirt or bending will reduce the sensitivity of your detector CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 6 Remove the screws that secure the lid then lift up the lid and set aside The top metal C ring and upper ceramic insulator may be attached to the lid 7 Remove the screws that secure the cover base then lift up the cover base ...

Page 222: ... the electrometer away from the detector to free the interconnect Turn the electrometer to the right to obtain working space Be careful not to touch or bend the spring Be careful not to lose the EMI suppressor 11 Remove the large metal C ring and the upper ceramic insulator if they were not attached to the lid 12 Remove the collector If the detector is operated at high temperatures the collector p...

Page 223: ...ese parts are stuck together do not separate them If they are not stuck remember which metal ring was on top of the insulator and which was below it The pieces must be reassembled in the same orientation Figure 46 NPD lower ceramic insulator and metal C ring 14 If not replacing the jet skip to step 21 15 Remove the column from the detector 16 Loosen the jet with a nut driver Metal C ring top Ceram...

Page 224: ...See Figure 45 25 Install the lid making sure that the NPD lid standoffs are in their slots Hold the lid flat while each of the screws is tightened until they touch the lid Tighten each screw evenly 1 2 turn at a time until tight Do not overtighten 26 Slide the electrometer interconnect into the slot on the lid and lower the electrometer into the mounting tray Be careful not to touch or bend the sp...

Page 225: ...lytical method 2 Turn Off the Bead Leave the NPD at operating temperature Leave flows on or off 3 Show the detector output signal in Status 4 Verify that the output leakage current is stable and 2 0 pA The output should slowly drop towards 0 0 pA and should stabilize in the tenths of a picoamp Current 2 0 pA indicates a problem ...

Page 226: ...nstalled plug the detector connection with the column nut and no hole ferrule Maintain inert carrier gas flow through the column or remove the column from the GC 5 Set normal operating flows 6 Set the detector temperature at 25 C above the typical method set point temperature 7 Set the oven temperature to 250 C or 25 C above the normal maximum operating temperature Do not exceed the column s tempe...

Page 227: ...o Replace the ECD Fused Silica Indented Mixing Liner and Install the Makeup Gas Adapter 233 To Install a Capillary Column in the ECD 236 To Bakeout the ECD 238 This section describes the routine maintenance tasks for the Electron Capture Detector ECD For important regulatory and safety information for this detector refer to the general information booklet and CD provided with the detector ...

Page 228: ...t is not exhaustive but indicates the kinds of compounds that may cause damage to 63 Ni detectors WARNING In the extremely unlikely event that both the oven and the detector heated zone should go into thermal runaway maximum uncontrolled heating in excess of 400 C at the same time and the detector remains exposed to this condition for more than 12 hours take the following steps After turning off t...

Page 229: ...s thoroughly with a mild nonabrasive cleaner after handling ECDs Cap the inlet and outlet fittings when the ECD is not in use Connect the ECD exhaust vent to a fume hood or vent it to the outside See the latest revision of 10 CFR Part 20 including Appendix B or the applicable state regulation For other countries consult with the appropriate agency for equivalent requirements Agilent Technologies r...

Page 230: ...2 3512 10 pk Ferrule graphite 1 0 mm id 0 53 mm capillary columns 5080 8773 10 pk Ferrule graphite 0 8 mm id 0 53 mm capillary columns 500 2118 10 pk Column nut finger tight for 0 53 mm columns Connect column to inlet or detector 5020 8293 320 Ferrule Vespel graphite 0 5 mm id 0 32 mm capillary columns 5062 3514 10 pk Ferrule graphite 0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5...

Page 231: ...1 3308 10 pk Capillary column blanking nut Testing use with any ferrule 5020 8294 Column nut universal Connect column to inlet or detector 5181 8830 2 pk Column cutter ceramic wafer Cutting capillary columns 5181 8836 4 pk Pencil diamond tipped Cutting capillary columns 420 1000 Ferrule tool kit Ferrule installation 440 1000 Table 37 Nuts ferrules and hardware for capillary columns continued Colum...

Page 232: ...ture Detector 232 Maintaining Your GC Exploded Parts View of the Electron Capture Detector Figure 47 Electron Capture Detector ECD exploded parts Column nut Makeup gas adapter Liner Cap Adapter nut Ferrules Warning tag Electrometer Perforated cover Makeup gas line ...

Page 233: ...es WARNING Be careful The oven and or detector may be hot enough to cause burns If the detector is hot wear gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds 3 Remove the column from the makeup gas adapter CAUTI...

Page 234: ... is broken or contaminated with sample or graphite 7 Ultrasonically clean the adapter cap in methanol Clean the outer surfaces of the makeup gas adapter with methanol 8 Install the fused silica indented mixing liner into the makeup gas adapter then install the cap The indentation on the fused silica indented mixing liner must be at the cap end of the adapter 9 Place a new 1 4 inch Swagelok nut and...

Page 235: ...e nut finger tight and then use a 9 16 inch wrench to tighten until snug If the adapter is properly installed the distance between the 1 4 inch nut and the bottom of the adapter will be 19 1 mm If the distance is 22 to 23 mm install the adapter into the detector fitting 12 Attach the column See To Install a Capillary Column in the ECD on page 236 13 Perform an inlet Leak Restriction test and reset...

Page 236: ...etector may be hot enough to cause burns If the detector is hot wear gloves to protect your hands WARNING Wear safety glasses to protect your eyes from flying particles while handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds 3 Load the inlet maintenance method and wait for the GC to become ready CAUTION Wear clean l...

Page 237: ...t stops at the indentation Pull it back 1 to 2 mm and tighten the column nut with one 5 16 inch wrench on the adapter and another 1 4 inch wrench on the column nut If the id is less the 200 um mark the column with a septum 70 1 mm from the end Insert column and nut into the adapter with the septum at the rear of the column nut and tighten the column nut with one 5 16 inch wrench on the adapter and...

Page 238: ... become ready to continue all zones cooled to safe handling temperatures 3 With the detector oven at normal operating temperatures show the detector output signal in Status Note the value of the Output for later comparison a On the GC touchscreen go to Home Status listing Add b Select Detector 1 Output or Detector 2 Output from the drop down list c Touch Add WARNING Be careful The oven and or dete...

Page 239: ...s The figure below shows detector output during a typical cleaning cycle 9 Check the ECD output value on the control table It should be lower than the first reading If it is not contact your Agilent service representative 10 Reinstall the column 11 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 12 Restore the analytical method ...

Page 240: ...14 Maintaining the ECD To Bakeout the ECD 240 Maintaining Your GC ...

Page 241: ...e FPD 242 Exploded Parts View of the Flame Photometric Detector Plus 244 To Install a Capillary Column to the FPD 245 To Change the FPD Wavelength Filter 247 To Remove the FPD Cover 250 To Replace the FPD Ignitor 251 To Install the FPD Cover 253 Cleaning the FPD Brazement 254 ...

Page 242: ...d column adapters 5180 4103 10 pk Ferrule Vespel graphite 1 8 inch for packed column adapters 0100 1332 10 pk Nut 1 4 inch brass for packed column adapters 5180 4105 10 pk Ferrule Vespel 1 4 inch for packed column adapters 5080 8774 10 pk 1 8 inch Packed column adapter assembly G3435 81340 1 4 inch Packed column adapter assembly G3435 81330 Preventive maintenance kit single FPD G3435 67000 Prevent...

Page 243: ...te 0 37 mm id 0 1 mm and 0 2 mm capillary columns 5062 3516 10 pk Ferrule Vespel graphite 0 4 mm id 0 1 mm 0 2 mm and 0 25 mm capillary columns 5181 3323 10 pk Ferrule graphite 0 5 mm id 0 1 mm 0 2 mm 0 25 mm and 0 32 mm capillary columns 5080 8853 10 pk Ferrule graphite 0 4 mm id 500 2114 10 pk Column nut finger tight for 100 to 320 mm columns Connect column to inlet or detector 5020 8292 All Fer...

Page 244: ...me Photometric Detector Plus FPD dual wavelength exploded parts Ignitor glow plug Capillary column nut Column ferrule Collar Screw Ignitor cable assembly Single wavelength FPD cover Filter Spacer for sulfur ﬁlter PMT assembly Adapter ferrule Adapter nut 1 8 inch Packed column adapter Spring Dual wavelength FPD cover Column measuring tool PMT assembly right usually with sulfur ﬁlter installed Sprin...

Page 245: ...e handling cutting or installing glass or fused silica capillary columns Use care in handling these columns to prevent puncture wounds CAUTION Wear clean lint free gloves to prevent contamination of parts with dirt and skin oils 3 Assemble a septum column nut and ferrule on the end of the column 4 Insert the end of the column through the column measuring tool so that the end protrudes beyond the t...

Page 246: ...pe the column walls with a tissue dampened with isopropanol to remove fingerprints and dust 10 Carefully thread the swaged column up into the detector fitting Finger tighten the column nut then use a wrench to tighten an additional 1 8 turn 11 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished Good Bad ...

Page 247: ...or Specifics then select the Photomultiplier High Voltage c If the voltage is enabled turn it off and apply the updated method d Return to the maintenance mode screen Maintenance Instrument WARNING Be careful The detector may be hot enough to cause burns If the detector is hot wear heat resistant gloves to protect your hands CAUTION The photomultiplier tube PMT is extremely sensitive to light Alwa...

Page 248: ...ace it face down 6 Place a clean cloth under the filter housing to catch the filter For phosphorus filter use the sharpened wooden tip of a toothpick or cotton swab to dislodge the filter from the housing For sulfur filter shown below use the wooden tip of the cotton swab to remove the filter spacer Then dislodge the filter from the housing ...

Page 249: ...lter and the arrow on the edge of the sulfur filter should face away from the flame and toward the PMT 8 Install the filter in the filter housing Install the sulfur filter spacer if necessary 9 Replace the PMT assembly and secure with the spring 10 Route the PMT wires through the clips as shown Avoid placing the wires very near heated areas such as the emission block or oven top 11 Exit maintenanc...

Page 250: ...the flame to prevent condensation from dripping into the jet and column WARNING Be careful The detector may be hot enough to cause burns If the detector is hot wear heat resistant gloves to protect your hands 3 Open the FPD detector top cover 4 Loosen the screws securing the FPD cover to the top of the detector 5 For a single wavelength FPD remove the two screws at the bottom left of the cover 6 L...

Page 251: ...nance Maintenance Mode Start Maintenance Wait for the GC to become ready WARNING Be careful The detector may be hot enough to cause burns If the detector is hot wear heat resistant gloves to protect your hands 3 Remove the FPD cover See To Remove the FPD Cover on page 250 4 Loosen the collet screw holding the cable assembly to the ignitor Remove the collet and cable assembly 5 Use a nut driver to ...

Page 252: ...he collet set screw as shown Do not let the collet screw touch metal parts such as the emission block or PMT bracket dual wavelength detector 8 Replace the FPD cover See To Install the FPD Cover on page 253 9 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 10 Restore the analytical method 11 Wait 20 min for the detector to heat up then ignite the f...

Page 253: ...owing T 20 Torx screwdriver 2 Install the cover Single wavelength detector a Start the two screws on the right side of the cover b Start and tighten the screws at the base on the left side c Tighten the screws on the right side Dual wavelength detector Install the cover two screws 3 Close the FPD detector top cover ...

Page 254: ...es necessary to clean the brazement to remove contamination note that exposing the inert coating to abrasives or certain solvents will degrade the coating If cleaning is needed follow the recommendations below for best results Rinse with a solvent appropriate to dissolve the expected contaminants Avoid abrasive or highly basic solutions see the caution above Recommended solvents dichloromethane ac...

Page 255: ...ts in the Aux EPC 258 Consumables and Parts for the PCM 260 Calibrating the PCM Interface 261 Installing or Replacing Frits in the PCM 262 This chapter describes the maintenance procedures for Auxiliary EPC Aux and Pneumatics Control Module PCM Pneumatic Switching Devices PSD do not have any required routine maintenance ...

Page 256: ...art number O rings package of 6 5181 3344 Blue dot frit high flow resistance G3430 80063 Red dot frit medium flow resistance G3430 80062 Brown dot frit low flow resistance G3430 80061 No frit brass tube zero flow resistance G3430 20011 Table 41 Auxiliary channel frits Frit marking Flow resistance Flow characteristic Often used with Three rings Blue High 3 33 0 3 SCCM 15 PSIG NPD Hydrogen Two rings...

Page 257: ...Aux EPC Maintaining Your GC 257 None brass tube Zero No restriction Headspace vial pressurization purged splitter and Deans Switch when using backflush Table 41 Auxiliary channel frits continued Frit marking Flow resistance Flow characteristic Often used with ...

Page 258: ...dot or Medium Red dot frit with hydrogen 2 Turn off the gas supply to the channel 3 To select the appropriate auxiliary channel frit See Table 41 4 Identify which frit needs to be changed Trace the tubing as needed to confirm 5 Remove the screw to the molded partner fitting 6 Lift the molded partner fitting away from the Aux EPC module 7 Remove the tubing weldment for the desired channel This will...

Page 259: ... 11 Restore gas flows and check for leaks at the fitting After installing or replacing a frit be sure to update the Aux EPC module PIDs used with your module If needed update the Aux EPC module PIDs using the GC Firmware Update Tool available on www agilent com To download the GC Firmware Update Tool open a web browser navigate to www agilent com then in the search box type in GC Firmware Update t...

Page 260: ...ee the Agilent catalog for consumables and supplies for a more complete listing or visit the Agilent Web site for the latest information www agilent com chem supplies Table 42 PCM consumables Description Part number O rings package of 12 5180 4181 Proportional valve Carrier G3430 67013 Proportional valve AUX G3430 67016 ...

Page 261: ...ting 2 Turn on the GC and wait 15 minutes to allow it to reach thermal equilibrium 3 When the GC has reached thermal equilibrium press Options scroll to Calibration and press Enter 4 Scroll to the module to be zeroed and press Enter 5 Scroll to a zero line and press Info The GC will remind you of the conditions necessary for zeroing that specific sensor Flow sensors Verify that the gas is connecte...

Page 262: ... appropriate frit 4 Remove the screw holding the partner fitting with the output tubing 5 Remove the tubing block Remove the frit and O ring using the tweezers Be careful to avoid scratching the metal surfaces 6 Remove the other O ring as well Replace it with a new O ring 7 Place a new O ring on the new frit and press it down into the block 8 Place the block on the module and tighten the screw fir...

Page 263: ...ARNING When hydrogen is used dangerously high flows are possible if insufficient flow resistance is provided downstream of the supply tube Always use either the High Blue dot or Medium Red dot frit with hydrogen After installing or replacing a frit be sure to update the PIDs used with your PCM ...

Page 264: ...16 Maintaining EPC Modules Installing or Replacing Frits in the PCM 264 Maintaining Your GC ...

Page 265: ... and Parts for Valves 266 Exploded Parts View of GC Rotary Valves 267 To Replace a Gas Sampling Valve Loop 268 To Align a Rotary Valve Rotor 270 To Replace a Rotary Valve in the Valve Box 271 To Remove the Upper Valve Box 274 To Install the Upper Valve Box 275 ...

Page 266: ...2 9509 10 port 400 psi 225 C maximum temperature 5062 9510 10 port Nitronic 60 300 psi 350 C maximum temperature 0101 0585 10 port Hastelloy 400 psi 225 C maximum temperature 5062 9511 Valves liquid sampling 0 2 µL 1000 psi stainless steel 175 C maximum temperature 0101 0636 0 5 µL 5000 psi 175 C maximum temperature 0101 0639 0 5 µL 1000 psi stainless steel 175 C maximum temperature 0101 0637 1 0 ...

Page 267: ... Parts View of GC Rotary Valves Maintaining Your GC 267 Exploded Parts View of GC Rotary Valves Figure 51 GC rotary valve exploded parts Rotor index pin Valve rotor Preload assembly Valve actuator Valve body Upper valve box assembly ...

Page 268: ...e line 4 Set all valve box valves to Off 5 Leave on the GC and valve actuator air 6 Turn off the carrier gas and sample line flows and relieve any back pressure to the valve WARNING The valve box insulation is made of refractory ceramic fibers RCFs To avoid inhaling RCF particles we recommend these safety procedures Ventilate your work area Wear long sleeves gloves safety glasses and a disposable ...

Page 269: ...nstall the new sample loop 11 Repressurize the sample loop and check for leaks 12 Install the upper valve box See To Install the Upper Valve Box on page 275 13 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 14 Restore the analytical method ...

Page 270: ...or and valve box may be very hot If they are hot wear heat resistant gloves to protect your hands 4 Loosen the adjustment set screw 5 Locate the rotor adjustment shaft on top of the actuator Using a flathead screwdriver rotate the valve rotor counterclockwise until it stops then back it off a small amount to set one end of the rotor s motion 1 mm 6 Tighten the adjustment set screw 7 Turn the valve...

Page 271: ... on the GC and valve actuator air 5 Turn off the carrier gas and sample line flows and relieve any back pressure to the valve WARNING The valve box insulation is made of refractory ceramic fibers RCFs To avoid inhaling RCF particles we recommend these safety procedures Ventilate your work area Wear long sleeves gloves safety glasses and a disposable dust mist respirator Dispose of insulation in a ...

Page 272: ...gs WARNING Hazardous sample gases may be present 13 Turn on the carrier and sample gases then check for leaks at the valve fittings Using the needle nosed pliers to toggle the valve check both the On and Off positions When leak free set the valve to Off See step 11 14 Install the upper valve box assembly See To Install the Upper Valve Box on page 275 15 Reset the valve EMF counters Valve rotor ind...

Page 273: ...in the Valve Box Maintaining Your GC 273 16 Perform an inlet Leak Restriction test and reset the maintenance counters 17 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished 18 Restore the analytical method ...

Page 274: ... to protect your hands 3 Lift and remove the detector cover 4 Remove the mounting screws from the upper valve box 5 Lift up and set aside 6 Exit maintenance mode Select Maintenance Instrument Perform Maintenance Maintenance Mode Finished WARNING The valve box insulation is made of refractory ceramic fibers RCFs To avoid inhaling RCF particles we recommend these safety procedures Ventilate your wor...

Page 275: ... valve box on top of the lower valve assembly routing the heater sensor wires through the cutouts Secure with two T 20 mounting screws 5 Push each coupling shaft assembly downward with a flathead screwdriver until the slot on the coupling engages the rotor index pin If the coupling and valve do not engage check that both are fully counterclockwise and try again If necessary turn the shaft slightly...

Page 276: ...17 Maintaining a Valve To Install the Upper Valve Box 276 Maintaining Your GC ...

Page 277: ...277 A Swagelok Connections Making Swagelok Connections 278 Using a Swagelok Tee 281 The gas supply tubing is attached with Swagelok fittings If you are not familiar with Swagelok connections review the following procedures ...

Page 278: ...lok nuts and ferrules 2 Clamp a stainless steel plug or similar fitting in a bench vise CAUTION Use a separate stainless steel fitting in a vise for initial tightening of the nut Do not use an inlet or detector fitting Strong forces are required to properly set the ferrules and damage to an inlet or detector fitting is very costly to repair 3 Push the tubing into the stainless steel plug See Figur...

Page 279: ...ut 7 Mark the nut with a pencil line See Figure 55 Figure 55 Mark the fitting 8 For 1 8 inch Swagelok fittings use a pair of 7 16 inch wrenches to tighten the fitting 3 4 of a turn See Figure 56 For 1 4 inch fittings use a pair of 9 16 inch wrenches to tighten them 1 1 4 turn as shown in Figure 56 Figure 56 Final tightening Front ferrule Back ferrule Nut Insert tubing fully Withdraw tubing 1 to 2 ...

Page 280: ...ther fitting finger tighten the nut then use a wrench to tighten it 3 4 1 8 inch fittings or 1 1 4 1 4 inch fittings of a turn 10 Both correctly and incorrectly swaged connections are shown in Figure 57 Note that the end of the tubing in a correctly swaged fitting is not crushed and does not interfere with the action of the ferrules Figure 57 Completed fitting ...

Page 281: ...ignal Materials needed 1 8 inch preconditioned copper tubing Tubing cutter 1 8 inch Swagelok nuts and front and back ferrules 1 8 inch Swagelok Tee Two 7 16 inch wrenches 1 8 inch Swagelok cap optional 1 Cut the tubing where you want to install the Tee Connect the tubing and Tee with a Swagelok fitting See Figure 58 Figure 58 Swagelok tee 2 Measure the distance from the Tee to the GC inlets Attach...

Page 282: ...www agilent com Agilent Technologies Inc 2019 First edition January 2019 G2790 90015 G3540 90015 ...

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