Emerson Rosemount FPD for Gas Chromatographs Hardware Reference Manual

7R00370-H01 Revision B October 2017 FPD for Gas Chromatographs Hardware Reference Manual Introduction NOTICE ROSEMOUNT (“SELLER”) SHALL NOT BE LIABLE FOR TECHNICAL OR EDITORIAL ERRORS IN THIS MANUAL OR OMISSIONS FROM THIS MANUAL. SELLER MAKES NO WARRANTIES, EXPRESSED OR IMPLIED, INCLUDING THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE, WITH RESPECT TO THIS MANUAL AND, IN NO EVENT, SHALL SELLER BE LIABLE FOR ANY SPECIAL OR CONSEQUENTIAL DAMAGES INCLUDING, BUT NOT LIMITED TO, LOSS OF PRODUCTION, LOSS OF PROFITS, ETC. PRODUCT NAMES USED HEREIN ARE FOR MANUFACTURER OR SUPPLIER IDENTIFICATION ONLY AND MAY BE TRADEMARKS/REGISTERED TRADEMARKS OF THESE COMPANIES. 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This limited warranty is the only warranty made by Seller and can be amended only in a writing signed by an authorized representative of Seller. Except as otherwise expressly provided in the Agreement, THERE ARE NO REPRESENTATIONS OR WARRANTIES OF ANY KIND, EXPRESSED OR IMPLIED, AS TO MERCHANTABILITY, FITNESS FOR PARTICULAR PURPOSE, OR ANY OTHER MATTER WITH RESPECT TO ANY OF THE GOODS OR SERVICES. It is understood that corrosion or erosion of materials is not covered by our guarantee. LIMITATION OF REMEDY AND LIABILITY: SELLER SHALL NOT BE LIABLE FOR DAMAGES CAUSED BY DELAY IN PERFORMANCE. THE SOLE AND EXCLUSIVE REMEDY FOR BREACH OF WARRANTY HEREUNDER SHALL BE LIMITED TO REPAIR, CORRECTION, REPLACEMENT, OR REFUND OF PURCHASE PRICE UNDER THE LIMITED WARRANTY CLAUSE IN SECTION 1 HEREIN. 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THE TERM “CONSEQUENTIAL DAMAGES” SHALL INCLUDE, BUT NOT BE LIMITED TO, LOSS OF ANTICIPATED PROFITS, LOSS OF USE, LOSS OF REVENUE, AND COST OF CAPITAL. Introduction Table of Contents Table of Contents 1 Introduction .......................................................................... 1 1.1 1.2 1.3 2 Setup................................................................................... 19 2.1 2.2 2.3 2.4 3 3.2 3.3 Model 500 FPD drawings ............................................................................................. 29 Model 700 FPD drawings ............................................................................................. 30 Enclosure threaded entry details ................................................................................. 51 Appendix B: Manufacturer’s manuals ..................................... 57 B.1 B.2 C Operation.................................................................................................................... 23 3.1.1 Igniting the flame manually ............................................................................. 24 Maintenance ............................................................................................................... 25 Troubleshooting.......................................................................................................... 26 Appendix A: Drawings .......................................................... 29 A.1 A.2 A.3 B Gas connections .......................................................................................................... 19 EnvironmentalConsiderations ..................................................................................... 19 Utility gases ................................................................................................................. 19 Venting ....................................................................................................................... 20 Operation and maintenance.................................................. 23 3.1 A Theory of operation ........................................................................................................2 Equipment description ...................................................................................................4 1.2.1 Model 500 FPD ...................................................................................................6 1.2.2 Model 700 FPD ...................................................................................................9 1.2.3 Model 700 FPD front entry ............................................................................... 12 1.2.4 Model 700XA FPD ............................................................................................ 13 1.2.5 Model 700XA FPD front entry .......................................................................... 14 1.2.6 Model 1500XA FPD .......................................................................................... 15 Glossary ...................................................................................................................... 16 FlamePhotometric Detector Operation Manual ........................................................... 58 GUB FPD 118500-3411 GUB ........................................................................................ 67 Appendix C: Spare Parts List ................................................ 107 i Introduction 1 Introduction The flame photometric detector (FPD) that you have received is factory-engineered to be used in conjunction with all Rosemount gas chromatographs. The FPD can be used as a solitary detector to measure low levels of sulfur compounds in natural gas or as a secondary detector in conjunction with a thermal conductivity detector (TCD) that allows the GC to analyze the full range of components present in a natural gas sample, including sulfur compounds. Figure 1-1: Flame Photometric Detector (FPD) A. Flame photometric detector (FPD) B. Photomultiplier tube C. Flame cell D. Electrometer board An FPD (A) typically consists of the following major components: The flame cell (C) - Located in the lower enclosure, the flame cell has connections for fuel gas, hydrocarbon-free air,sample injection (process gas plus nitrogen carrier), and an exhaust pipe. It is fitted with an RTD to monitor the temperature when running, and an ignitor to light the fuel gas. The photomultiplier tube (B) - Located in the lower enclosure, the photomultiplier tube contains the sensors that measure the light that is emitted from the flame cell during operation. It has one signal lead and one high voltage wire that take the signal from the detector to the electrometer board and provide the power for ignition. The leads are co-axial typecables. 1 Introduction The electrometer board (D) - Located in the upper enclosure, the electrometer board amplifies and processes the signal data from the detector, and sends it to the CPU board on the GC. It also provides the ignition circuit, controls the re-light function, and generates the flame out alarm. 1.1 Theory of operation NOTICE See also Section 1.3 of this manual, for definitions of some of the terminology used in the following explanations. The detection system in the FPD uses the reactions of sulfur components in a hydrogen or air flame as a source for analytical detection. The source of the FPD's signal is derived from the light produced by an excited molecule created in the flame's combustion, which is a photochemical process called chemiluminescence. A thermocouple is fitted to the flame cell to ensure that the flame is present. If the flame is not detected, the electrometer shuts off the hydrogen to the flame cell. It then supplies a voltage to the igniter, waits five seconds and opens the hydrogen shut off valve. The electrometer will make ten ignition attempts if necessary. If it is not successful, then the hydrogen is shut off, an alarm is triggered on the GC and the unit awaits attention from the operator. NOTICE To ignite the flame manually, see Section 3.1.1. The signal is sent from the PMT to the electrometer to be amplified. The electrometer also provides the PMT with the high voltage it requires to operate the auto re-light circuits.1.3 2 Introduction Figure 1-2: Elution of Components 1. Carrier gas only at the detector 2. First component begins to elute from the columns and is sensed by the detector. 3. Peak concentration of first component. 4. The second component begins to elute from the columns and is sensed by the detector. 5. Peak concentration of the second component. 3 Introduction The signal is then sent to the preamplifier board for further amplification. In addition, the preamplifier converts each voltage signal to a value that is proportional to the concentration of the component detected in the gas sample. The preamplifier provides four different gain channels as well as compensation for baseline drift. The signals are sent to the GC for computation or for viewing on a PC monitor or local operator interface (LOI). While the GC is in Idle mode, prior to injecting a sample, the detector is exposed to pure carrier gas. In this condition, the output from the detector is electrically nulled. The detector output is set to 1 mV DC. This is measured on the red and black terminals on the preamplifier board, and adjusted using the potentiometer (R38) on the electrometer PCB. 1.2 Equipment description FPDs are available in the following configurations: • Model 500 FPD • Model 700 FPD • Model 700 FPD Front Entry • 700XA FPD • 700XA FPD Front Entry • 1500XA FPD NOTICE The Front Entry configurations include an additional frame to allow all the FPD enclosures to be mounted on the front of the unit. This allows the unit to be located close to a wall because no rear access is required for installation or maintenance. All configurations are ATEX-certified. The differences between the configurations are detailed in later sections of this chapter. 4 Introduction The FPD used with the Model 500, 700, and 700XA gas chromatographs has the following hazardous area certification markings: 5 Introduction 1.2.1 Model 500 FPD Figure 1-3: Model 500 FPD The Model 500 FPD module consists of three Exd GUB enclosures mounted on a frame, plus an Exd solenoid that acts as a hydrogen shut-off valve. The enclosures contain the following: 6 • Electrometer assembly in GUB 5 enclosure • Flame cell and photometric detector tube in GUB 5 enclosure • Transformer (either 230/110 Vac or 110/110 Vac) in GUB 4 enclosure • Hydrogen shut-off valve Introduction Figure 1-4: Model 500 FPD Enclosures A. Electrometer assembly B. Flame cell and FP tube C. H2 shut off valve D. Transformer Place the FPD module as close as possible to its partner GC to minimize the length of sample tubing between them, and therefore to keep the cycle time as short as possible. The tubing required to operate the FPD flame cell is 1/16 in. OD 0.010 in. ID. All tubing enters the GUB enclosure containing the flame cell via a specially designed tubing gland. All internal fittings are Swagelok double ferrule type compression fittings. 7 Introduction Figure 1-5: Specialized Tubing Gland 8 Introduction 1.2.2 Model 700 FPD Figure 1-6: Model 700 FPD The Model 700 FPD module consists of four Exd GUB enclosures mounted on a frame, plus an Exd solenoid valve that acts as a hydrogen shut-off valve. The Model 700 FPD requires an additional enclosure to house temperature control equipment that on a Module 500 GC is available internally. 9 Introduction The enclosures contain the following: • Electrometer assembly in GUB 5 enclosure • Flame cell and photometric detector tube in GUB 5 enclosure • PID Temperature controller and relay • Transformer (either 230/110 Vac or 110/110 Vac) in GUB 4 enclosure • Hydrogen shut-off valve Figure 1-7: PID Temperature Controller and Relay Place the FPD module as close as possible to its partner GC to minimize the length of sample tubing between them, and therefore to keep the cycle time as short as possible. The tubing required to operate the FPD flame cell is 1/16 in. OD 0.010 in. ID. All tubing enters the GUB enclosure containing the flame cell via a specially designed tubing gland. All internal fittings are Swagelok double ferrule type compression fittings. 10 Introduction Figure 1-8: Specialized Tubing Gland 11 Introduction 1.2.3 Model 700 FPD front entry Figure 1-9: Model 700 FPD Front Entry The Model 700 FPD front entry is comprised of the same components as the standard Model 700 FPD with an additional frame added to allow all the enclosures to be mounted on the front of the unit. This allows the unit to be located close to a wall because no rear access is required for installation ormaintenance. 12 Introduction 1.2.4 Model 700XA FPD Figure 1-10: Model 700XA FPD The Model 700XA FPD consists of four explosion-proof enclosures mounted on a frame plus an explosion-proof solenoid valve that acts as a hydrogen shut-off valve. 13 Introduction The enclosures contain the following components: • Electrometer assembly • Flame cell and photometric detector tube • Transformer, either a 230/110 Vac or a 110/110 Vac • PID temperature controller and relay • Hydrogen shut-off valve Place the FPD as close as possible to its partner GC to minimize the length of sample tubing between them, and keep the cycle time as short as possible. The tubing size required to operate the FPD flame cell is 1/16 in. OD 0.010 in. ID. All tubing enters the flame cell’s enclosure through a specially designed tubing gland. All internal fittings are Swagelok double ferrule compression fittings. Figure 1-11: Specialized Tubing Gland 1.2.5 Model 700XA FPD front entry The Model 700XA FPD front entry is comprised of the same components as the standard Model 700XA FPD with an additional frame added to allow all the enclosures to be mounted on the front of the unit. This allows the unit to be located close to a wall, because no rear access is required for installation or maintenance. 14 Introduction 1.2.6 Model 1500XA FPD Figure 1-12: Model 1500XA FPD The Model 1500XA FPD consists of four explosion-proof enclosures mounted on a frame plus an explosion-proof solenoid valve that acts as a hydrogen shut-off valve. The enclosures contain the following components: • Electrometer assembly • Flame cell and photometric detector tube • Transformer, either a 230/110 Vac or a 110/110 Vac • PID temperature controller and relay • Hydrogen shut-off valve 15 Introduction Place the FPD as close as possible to its partner GC in order to minimize the length of sample tubing between them, and therefore to keep the cycle time as short as possible. The tubing size required to operate the FPD flame cell is 1/16 in. OD 0.010 in. ID. All tubing enters the flame cell’s enclosure through a specially designed tubing gland. All internal fittings are Swagelok double ferrule compression fittings. Figure 1-13: Specialized Tubing Gland 1.3 Glossary Auto Zero Automatic zeroing of the preamplifier. May be entered into the controller to take place at any time during the analysis when either the component is not eluting or the baseline is steady (not normally used). Chromatogram A permanent record of the detector output. A chromatograph is obtained from a PC interfaced with the detector output through the GC controller. A typical chromatogram displays all component peaks and gain changes. It may be viewed in color as it is processed on a PC VGA display. Tick marks recorded on the chromatogram by the GC Controller indicate where timed events takeplace. Component Any one of several different gases that may appear in a sample mixture. For example, sample gas usually contains the following components: ethyl mercaptan, t-butyl mercaptan, methyl ethyl sulphide, diethyl sulphide, hydrogen sulphide, and carbonyl sulphide. 16 Introduction Response Factor Correction factor for each component as determined by the calibration. It is defined by the equation: where ARFn = Area response factor for component n in area per mole percent (%) HRFn = Height response factor for component n Arean = Area associated with component n in calibration gas Htn = Height associated with component n in mole % in calibration gas Caln = Amount of component n in mole % in calibration gas Retention time The time in seconds that elapses between the start of analysis ( 0 seconds) and the sensing of the maximum concentration of each component by the analyser detector. 17 Introduction 18 Setup 2 Setup 2.1 Gas connections 2.2 ® Use Silcosteel or equivalent tubing for all calibration gas and process gas connections on all FPDs that are used to measure low range sulfur components. If you use Grade 316 or other stainless steel piping, the sulfur components will adhere to the internal surface of the pipe, and will continue to do so until the entire internal surface of the tubing is coated or conditioned, which will result in lower than expected levels of sulfur components reaching the detector for measurement. Conditioning may take one week or longer, depending on the levels of sulfur components and the length of the tubing. Environmental Considerations FPDs are sensitive to changes in temperature and pressure; therefore, place them in shelters that have stable temperature and pressure. Do not use positive pressurization for shelters. 2.3 Utility gases FPDs require the following utility gases: • Hydrogen - 99.995% purity • Hydrocarbon-free air • Nitrogen - 99.995% purity (carrier gas) • Helium - 99.995% purity (optional second carriergas) 19 Setup ® Make all utility and process gas connections with Swagelok 1/8-inch double ferrule compression fittings. Metric conversion kits are available; contact your Rosemount sales representative for more information. These are typical values supplied for information only. Actual values are application specific. Figure 2-1: Typical Pressure and Flow Rate Information 2.4 Venting All Rosemount FPD modules have a vent from the flame cell that exits the GUB enclosure via a proprietary Exd breather/drain/ flame arrestor assembly. The exhaust from the flame cell emits water vapor as a result of burning hydrogen as fuel. This vapor condenses in the exhaust tubing outside the GUB enclosure, and can be seen as drips of water. Vent the FPD exhaust to atmosphere. Do not subject the vent to any back pressure because this will have a detrimental effect on the detector, and may cause the flame to extinguish. 20 Setup WARNING Hydrogen-air mixtures can ignite with very low energy input. For reference, an invisible spark or a static spark from a person can cause ignition. Although the auto- ignition temperature of hydrogen is higher than those for most hydrocarbons, hydrogen's lower ignition energy makes the ignition of hydrogen–air mixtures more likely. Use a container with the FPD module to collect the condensed water from the FPD vent. Do not pipe the vent away unless you can guarantee a continuous downward slope on the pipe and no back pressure or obstruction by water. 21 Setup 22 Operation and maintenance 3 Operation and maintenance 3.1 Operation The FPD operates as a separate detector. It is controlled by and reports to the GC. The flow rates for the utility gases and the carrier gas are factory set, and are specific to each FPD. These should only be adjusted by fully trained and authorized personnel. The FPD is identified as Detector #1 on the Detector screen, which is viewable with MON2000, MON2020, and the LOI. When used in conjunction with a TCD, the FPD is Detector #1, and the TCD is Detector #2. NOTICE The electrometer switch (A), which has three positions—up for Reset, centered for Normal, and down for Override—should not be left in Override. A. Electrometer switch 3-1 23 Operation and maintenance 3.1.1 24 Igniting the flame manually 1. Connect air to the inlet and slowly bring the inlet pressure to 60 psig. 2. Connect hydrogen to the inlet and slowly bring theinlet pressure to 60 psig. 3. Remove tubing from flame cell exhaust and use a digitalflow meter to adjust the air control valve until a reading of 160 cc/ min is obtained. 4. Turn off the air supply. 5. Set the auto relight switch (S1) on the electrometer PCB to the OVERRIDE position. 6. Use the digital flow meter to adjust the hydrogen controlvalve until a reading of 100 cc/min is obtained. 7. Turn on the air supply. 8. Set the auto relight switch (S1) on the electrometer PCB to the RUN position. The auto relight sequence starts as follows: a. The LED on the electrometer comes on after 10 seconds, and the glow plug fitted to the side of the flame cell is now supplied a voltage. b. After another 5 seconds, the hydrogen shut off valve operates. c. The gas mixture is ignited. d. If the flame does not light in 5 seconds, the electrometer de-energizes the hydrogen shut off valve to stop the flow into the flame cell. e. The flame cell is then purged with air and nitrogen carrier. f. The process starts again—up to 10times—until the flame stays lit. Operation and maintenance g. If the flame does not stay lit, the LED flashes. If the alarm output is linked to the 2350A controllerdiscreet input, there will be an alarm present on the controller. h. Set the auto relight switch (S1) on the electrometer PCB to the RESET position and then back to the RUN position. The re-light sequence isrestarted. If the unit still fails to light after resetting the electrometer, recheck the air and hydrogen flows. 3.2 Maintenance The FPD is a complex piece of equipment and needs to be regularly maintained, preferably as part of an annual planned maintenance process. The following important maintenance procedures should be conducted on an annual basis: Replace the flame cell and photometric tube O-rings, except for the Kalrez O-ring, which should be replaced every 24 months. • CAUTION Be certain that the flame cell has cooled down before touching it, because it often reaches a temperature of 170 °C (338 °F). • Lubricate the stem of the hydrogen shut-offvalve. For both of these operations, the GC should be shut down, and the appropriate permits and permissions gained before commencing. Only trained and authorized personnel should carry out maintenance.. NOTICE The flame out logic should always be tested to ensure it works at the end of any maintenance. Failure to maintain the FPD may cause a loss of functionality and can result in permanent damage to the equipment. 25 Operation and maintenance 3.3 Troubleshooting Only competent trained personnel should troubleshoot FPDs. The following list of faults is not definitive. It only details the most common faults. Fault symptom(s) • Check high voltage is present on coax. • Approx. -600 Vdc • If voltage now present on board, check coax cable. • Check BNC coax connectors are tight. If voltage is present, check signal coax. • If there is no voltage, or the signal cable is OK, replace electrometer. Upsets are being seen, but there are no peaks when gas is injected. • Check the 12 V GND wiring to the electrometer board. The two GND terminals on connector #2 are not linked on board. If there are three black wires, ensure that pins 1 and 4 are connected to the power supply. The other wire is for the flame cell GND. • Check the tubing going into the bottom of the flame cell. Loosen fitting and pull tubing downwards while watchingCGM. • If peaks appear, then the tubing needs to be cut. • Check to see if there is flow from the metering valve next to the heater block. • Check the sample is getting to the flame cell. • Try replacing the columns one at a time. • Check you are getting carrier through port 1 with valve 2 on and through port 5 with valve 2 off. If not check the vents on the Alcon valve for back pressure. When monitoring the baseline in MON2020, there are no upsets present when the auto re- light circuit fires. If no voltage, remove coax connector. 26 Possible solution(s) Operation and maintenance Fault symptom(s) Air and H2 flows are set correctly, and the unit fails to stay lit. Possible solution(s) • Using a digital thermometer connected to the thermocouple wires coming from the bottom of the flame-cell, check that the temperature is 160 °C (320 °F). • Check flame out thermocouple wires. • Ensure no insulation is trapped under screw on terminalstrip. • Try pulling the sample tube out when it is attempting to light in case the tube is affecting the fuel mixture. • Replace the flame cell and try again. • Ensure that the signal wires are connected to the correct place; remember that the white signal wire should be connected tothe TC+ of the CON5. Unit give good size sample peaks; then after a while, the peaks are not present, but the relight still gives good peaks. There might be soot on the sample tube going to the flame-cell. Pull tube down slightly while watching the CGM to see if that cures the fault. Flame cell temperature cannot be controlled. Check the flame cell thermistor. The resistance is approximately 100 KΩ at ambient. Resistance goes down as temperature goes up. • Check that the thermistor has not been pushed right through the flame cell. • In later models, the flame cell will be blanked at end of holes to ensure that this cannot happen. • Check there is enough heat-sink compound fitted around sensors. • Check the BNC connectors for the signal in and the high voltage. Ensure that they are tight. • Cut off the flame and check the response from the detector on a live CGM. • Try changing the filter. Restrictor metering valve seems to be restricting the output flow completely. • Apply Snoop® to the two fittings at the bottom of the metering valve. • Change the metering valve. Peaks are very small or appear to be back to front. • Check nitrogen flow into union at flame cell. • This should be no less than 15cc/min. Flame cell temperature is erratic. Unable to balance the bridge. 27 Operation and maintenance 28 Fault symptom(s) Possible solution(s) Noisy baseline and/or very big dips on the baseline. Check the air supply, which should be no lower than 500psi in the cylinder. Appendix A: Drawings A Appendix A: Drawings A.1 Model 500 FPD drawings DUK 7233/013/1 General Arrangement: Model 500 FPD Module DUK 7233/002/1 General Arrangement: Model 500 FPD Analyzer DUK 7233/039/1 General Arrangement: Model 500 FPD Dual Analyzer DUK 7233/028/1 Power Wiring Diagram: 500 FPD C/W Aux Stream Switching DUK 7233/029/1 Wiring Diagram: FPD Relight Failure Alarm DUK 7233/030/1 Power Wiring Diagram: Model 500 FPD DUK 7233/033/1 Interconnection Diagram: 500 FPD / 2350A Controller DUK 7233/034/1 Wiring Diagram: 500 FPD / 2350A Controller DUK 7233/048/1 Wiring Diagram: 500 FPD / 2350A – 6 x 6 Port Valves DUK 7233/056/1 Power Distribution : 500 FPD Dual Analyser C/W 2 x Trace Heat DUK 7233/062/1 Wiring Diagram : 500 FPD / 2350A – 6 x 6 Port – Aux Stream Switching NOTICE Flow Diagrams: Refer to the sales order documentation that was shipped with the GC. 29 Appendix A: Drawings A.2 Model 700 FPD drawings DUK 7204/074/1 General Arrangement: 700 FPD Analyzer DUK 7204/100/1 General Arrangement: 700 FPD Module DUK 7204/156/1 General Arrangement: 700 FPD Module Front Entry DUK 7204/102/1 Internal Cable Wiring: 700 FPD Analyzer DUK 7204/103/1 Power Wiring Diagram: 700 FPD Analyzer NOTICE Flow Diagrams: Refer to the sales order documentation that was shipped with the GC. 30 Appendix A: Drawings 31 Appendix A: Drawings 32 Appendix A: Drawings 33 Appendix A: Drawings 34 Appendix A: Drawings 35 Appendix A: Drawings 36 Appendix A: Drawings 37 Appendix A: Drawings 38 Appendix A: Drawings 39 Appendix A: Drawings 40 Appendix A: Drawings 41 Appendix A: Drawings 42 Appendix A: Drawings 43 Appendix A: Drawings 44 Appendix A: Drawings 45 Appendix A: Drawings 46 Appendix A: Drawings 47 Appendix A: Drawings 48 Appendix A: Drawings 49 Appendix A: Drawings 50 Appendix A: Drawings A.3 Enclosure threaded entry details DUK 7233/060/3 FPD Module Bottom Housing Assembly DUK 7233/061/3 FPD Module Top Housing Assembly DUK 7204/101/3 Model 700 FPD Module Temperature/Controller Enclosure DUK 7233/007/3 FPD Module Transformer Housing Assembly 51 Appendix A: Drawings 52 Appendix A: Drawings 53 Appendix A: Drawings 54 Appendix A: Drawings 55 Appendix A: Drawings 56 Appendix B: Manufacturer’s manuals B Appendix B: Manufacturer’s manuals • Flame Photometric Detector Operation Manual • PID Controller Manual 57 Appendix B: Manufacturer’s manuals B.1 FlamePhotometric Detector Operation Manual 23332-K026 Revision B April 25th, 2008 Information disclosed herein may not be reproduced in any form without the express permission of GC EXPRESS. 58 Appendix B: Manufacturer’s manuals IMPORTANT In order to obtain optimum performance from this detector, it is necessary to meet and maintain the following conditions: A. The following minimum purity standard for gases and liquids shall be maintained: Helium - 99.999% (ultra high purity) or Nitrogen - 99.999% (ultra high purity) Hydrogen 99.999% (ultra high purity) Air - 0.1 PPM total Hydrocarbons (ultra zero grade) B. Stainless steel diaphragm regulators must be used. C. All gas lines from source to instrument must be clean. B.1.1 General Description Introduction The Flame Photometric Detector, FPD, is a very sensitive and selective detector for the analysis of sulfur or organophosphorus containing compounds. The detector is very stable and easy to use. As the analyte is burned in a hydrogen and air flame, a characteristic wavelength of light is emitted at 394 nm for sulfur and 526 nm for phosphorus. A filter specific to the appropriate wavelength may be installed to enhance the selectivity to the sulfur or phosphorus emission. The emitted light is amplified by the photomultiplier tube (PTM) and processed by the signal processor. 'The response to phosphorus is linear and quadratic to sulfur. The detector may be operated in either the sulfur mode or phosphorus mode by switching the filter and adjusting the air to hydrogen ratio to optimize response. A shielded flame design of the detector enhances sensitivity by lowering the noise created by the light emitted by the flame. The detector uses a stainless steel jet, quartz windows, and silicone 0-rings in an all aluminum body. 59 Appendix B: Manufacturer’s manuals Specifications • Maximum operating temperature: 250 °C • Shielded stainless steel jet • Sensitivity: 2 x 10·12 g/sec for sulfur • Sensitivity: 1 x 10·12 g/sec for phosphorus • Linear range: l 04 for phosphorus • Linear range: 103 with optional square root function for sulfur • Leak tight design to allow measurement of all flows from detector exhaust • Igniter voltage: 1.5V AC at 4 amps • PMT voltage variable from approximately 650V Installation of the FPD Optical filter In order to have the specificity for sulfur or phosphorus detection the appropriate optical filter must be in place. The phosphorus filter is a filter of 526 nanometers and the sulfur is a filter of 396 nanometers. Before changing the filter, the power cable to the photomultiplier tube, PMT, must be removed. This will prevent irreparable damage which can be caused by the introduction of room light to the PMT. The two thumb screws securing the PMT to the detector body are removed and then the PMT is slid off gently. Some resistance is felt due to the O-ring on the detector body which provides a light tight seal. The filter may be removed and replaced with the appropriate filter. The sulfur filter is a very dark blue color and the phosphorus filter a fluorescent yellow green. One side of the filter has a mirror finish. There is not a front or back face to the filter. The PMT is slid back in place and the two thumb screws secured to the detector body. Reattach the power mid signal cables to the back of the PMT. 60 Appendix B: Manufacturer’s manuals Figure B-1: Insertion of Capillary Column into the FPD Operation CAUTION When working with the detector, never remove the photomultiplier from the detector with the dynode voltage applied. Exposure to high light levels will cause photocathode fatigue (sensitivity loss for an extended period of time) and may cause permanent damage. Optimal detector temperature The FPD may operate up to a temperature of 250 °C. Take care to operate the detector above the final temperature of the column to prevent the condensation of column bleed on the surface of the optical windows which could result in loss of response. CAUTION Do not operate the detector above 250 °C or you may damage the plastic photomultiplier housing. Optimizing flows and igniting the flame The optimization of the detector is achieved by adjusting the ratio of hydrogen to air. The oxygen content of air should be 0.2 - 0.4 of the hydrogen flow, with the optimum ratio being 0.3. The air flow should be 1.5 times the hydrogen flow. When optimizing conditions, the higher the total gas flows; the higher the background noise. 61 Appendix B: Manufacturer’s manuals Example: Hydrogen flow 100 mL/min 100 mL/min x 1.5 = 150 mL/min air required Nitrogen is the most common carrier gas used for packed columns. Helium is used for the carrier gas for capillary column s with nitrogen for the make-up gas. Once the flows are set and the detector is at a temperature of at least 125 °C, the flame may be lit. Selecting the Linear or Square Root Mode of Operation The FPD electrometer has two modes of operation designated as" linear" and "square root". To select the mode of operation, use the sq rt / linear switch. In the linear mode, the circuit performs as a basic electrometer giving a 10 volt output for an input current of one microampere. This 10 volt full scale output is available at the 10 volt output. A 1 volt output is also available. The linear mode is used when the detector is operated in the phosphorus mode of operation with the phosphorus filter installed. Phosphorus is detected as POH. 62 Appendix B: Manufacturer’s manuals Sulfur is detected as S2 and the response is proportional to the square of the concentration of the sulfur containing compound. The square root mode is selected from the switch marked sq rt / linear. In this mode the electrometer output is modified by a special resistordiode matrix to correct for the non-linear (approximately square law) relationship between the detector output current and sulfur concentration when the detector is operated in the sulfur mode. When operating in the mode, the electrometer zero control should be set to provide a slightly positive output from the module with the detector output at baseline. Figure B-2: Replacement of O-rings and Windows 63 Appendix B: Manufacturer’s manuals Maintenance CAUTION When working with the detector, never remove the photomultiplier from the detector with the dynode voltage applied. Exposure to high light levels will cause photocathode fatigue (sensitivity loss for an extended period of time) and may cause permanent damage to the PMT. Cleaning the Detector Column bleed may build up in the FPD housing. This stationary phase coating may be rinsed out of the detector without disassembly. Follow the procedure listed below: 1. Disconnect the electrical connections from the detector. 2. Tum off the hydrogen and air supply lines to the GC. 3. Cool the detector to ambient. 4. Disconnect the column, hydrogen and air lines from the detector body. 5. Remove the detector from the GC. 6. Cap the hydrogen and air inlets with an 1/8" cap nut. 7. Flush the detector thoroughly with acetone through the column inlet port and exiting through the exhaust tube. 8. Dry the detector with nitrogen thoroughly. 9. Uncap the gas inlets and reinstall the detector onto the GC. Replacing the O-rings and Quartz Windows After using the detector for about twelve months at 250° or more, the O -rings may become brittle and begin to allow light to leak into the detector resulting in high background noise and loss of response. The quartz window may need to be replaced as well. There are a total of five O-rings in the O-ring replacement kit, PIN 116910-KAL REZ. Four are Kalrez and one is Teflon. The locations of these O- rings are shown in Figure B-2. These O -rings must be replaced any time a joint sea led by one of them is separated. ' The cross section view of the detector is shown in Figure B-2. There are two concentric O-rings between the window housing and flame base. A 1-1/4" Kalrez ring fits into a groove in the window housing itself and a 15/16" Teflon ring fits around a bushing between the window and the flame base. A 15/16" Kalrez ring is used between the window at the inner end of the filter housing and the heat radiator section. The following procedure should be used to replace the O -rings and quartz windows: 1. Disconnect the power cable from the PMT. 2. Loosen the two thumb screws on the filter housing and remove the PMT. 3. Remove the filter. 4. With a Phillips screwdriver, disconnect the heater-igniter wiring bracket from the housing assembly. 5. Pull the filter housing from the recess in the heat radiator, exposing first the window and O-ring (15/16 in. Kalrez). 6. With a hex (Allen) wrench, remove the four screws holding the radiator and window housing to the flame base. 7. Remove the heat radiator, window housing, and the window 8. Remove the old O-rings. 64 Appendix B: Manufacturer’s manuals 9. Place the 15/16 in. Teflon ring around the metal bushing. 10. Insert the 1-1/4-in. ring into the groove in the window housing. 11. With the bushing and its ring between the window and the flame base and grooved side of the window housing toward the flame base, align the window housing with the threaded holes in the flame base. 12. Replace the heat radiator over the window housing with countersunk holes toward the outside and aligned with the holes in the window housing and flame base. 13. Replace the Allen head screws and tighten. 14. Place the outer window in the recess in the inner end of the filter housing with the 15/16in. Kalrez O-ring between the window and the heat radiator. 15. Replace the filter housing and the wiring bracket. 16. Replace the filter and the PMT. The 1 -1/4-in. Kalrez end cover O-ring is located between the end cover and the flame base. Recommended spare parts The figure below is a cross-section diagram of the FPD with associated part numbers. The parts listed below are used in the normal maintenance of the detector. Description Part number Igniter plug (includes O-ring seal) – 1.5 volt 116906-K001 Quartz window 23608-0019 O-ring kit 2 ea. # 2-27 Kalrez (1.437 O.D. x 0.70 dia cross section) 1 ea. #2-21 Kalrez (1.062 O.D. x 0.70 dia cross section) 1 ea. #c2118-021 PFTE (1.062 O.D. x 0.70 cross section) 1 ea. #568-010 Kalrez O-ring # S70010 ignitor 1 ea. #586-011 Kalrez O-ring #S70011 flame out TC 116910-KALREZ 65 Appendix B: Manufacturer’s manuals 66 Appendix B: Manufacturer’s manuals B.2 GUB FPD 118500-3411 GUB 67 Appendix B: Manufacturer’s manuals B.2.1 Full function uP controlled FPD Rev G 1. FPD Processor Control Functions A. Power on Initialization. B. Reset State. The uP monitors the RESET/RUN/OVERRIDE Switch (R/R/0 Switch) (SW1), suspending any automatic operation until the R/R/ 0 Switch is set to the RUN position. If the R/R/0 Switch is set to the Override position, the uP continues to be Reset but the fuel valve will be manually activated . The fuel valve will remain activated until the R/R/0 Switch is manually switched to either the Reset or Run position. C. Igniter and Flame on State. When the R/R/ 0 Switch is set to the R UN position, the uP attempts to ignite the flame. Tl1e ignition sequence consists of the following steps. 1. Tum the Igniter Drive and LED (D20) on and wait for 5 sec. This allows the igniter to reach a temperature that will cause ignition. 2. Open the fuel valve and wait for 15 sec. 3. Tum the Igniter Drive and LED off. 4. Check for Flame On by monitoring the thermocouple temperature sensor input at connector CON5. 5. If no flame is detected, fuel valve will be closed and the uP will delay for another 30 sec. before any attempt to retry the ignition sequence. 6. lf a flame is detected, the uP will continue monitoring the thermocouple temperature sensor input for a flame on indication, maintaining the fuel valve on and the LED indicator off. If the uP does not detect a flame within 10 tries of the Ignition Sequence, it will set the igniter and fuel solenoid off and indicate a error condition by flashing the LED indicator (D20) at a steady 2Hz. An external error control signal (External Alarm), which can be used to drive a remote indicator (LED, Buzzer, Etc.), will be activated at connector CON3.l. The uP will suspend any other operation until the R/ R/0 switch has been cycled off and back on or the power has been cycled off and back on. The uP will enter the Ignition Sequence and will attempt ignition: a. On power up if the R/R/0 Switch is set to RUN. b. Anytime the R/ R/0 Switch is cycled from RESET or OVER RIDE to RUN. c. In nominal operation , whenever the flame has been on and has gone out. If the flame cannot be started within 10 tries of the Ignition Sequence , the uP will not try to re-ignite until the R/R/0 Switch has been manually cycled off and back on or the power has been turned off and back on. Any time the R/R/0 Switch is cycled from RUN to RESET, the uP will stop fuel flow by turning the fuel solenoid off. No attempt will be made to restart the flame until the R/ R/0 Switch is returned to the RUN position. Warning: The R/R/0 Switch is a three-position switch, and once switched to the OVERRIDE position there is no automatic termination of the fuel valve activation. This feature is used for set.up of the fuel flow only. To deactivate the fuel valve, the R/R0/ Switch must be manually switched back to the RUN or RESET positions. Refer to FPO Firmware Flowchart for detailed outline of uP functions. 68 Appendix B: Manufacturer’s manuals 2. FPD Electrometer Power Supply: Use caution. AC Voltage (120 Volts AC) is present and DC Voltage in excess of 600 Volts is generated on the PCB when power is applied. A. Extemal Power, AC Volts: 120 Volts AC routed thru CON4 is switched by the Solid State Relay U7 (S101DH2). The Gas Valve/Solenoid is controlled by this switched AC Voltage signal. B. External Power, DC Volts: 12 Volt DC to low voltage power connector CON2. CON2, Pins I & 2, power the low current section of the PCB. CON2, Pins 3 & 4, power high current circuits (HV Regulator, Igniter, fuel solenoid, etc.). C. On board low voltage: 1. An on board DC to DC Converter (U6) generates +/- 15 Volts 2. A LM4040 Voltage Regulator (U5) generates +5 Volts D. On board high voltage: On board high voltage converter generates approximately 650 Volt DC (J4) 3. FPD Linear Mode Test A. Set the Linear / Sq. Root Switch (SW3) to Linear Mode B. During the following test steps, monitor U3.6 output line with an oscilloscope to check for oscillation or other signs of faulty operation. C. With Signal In input connector (J3) open, recorder span set to 1 mV. full scale and the Zero Switch (SW4) set to OFF, adjust R57 for best output null. D. With Signal In input connector (J3) open, set the Zero Switch (SW4) ON. Adjust the manual zero pot (R38, can be located on the PCB or mounted on the front panel) completely CW and check for an output of +0.055V to +0.075V. Adjust the zero pot completely CCW and check for a smoothly changing voltage output to - l. l 5V to -1. 55V. Return the Zero voltage control to approx. 0 volts output. E. Connect a current source to the Signal In input connector (J3). With a Voltmeter or recorder, monitor the output at the l OV output pin (CON I. 4). Change recorder span as necessary to check output range and linearity per following table. Current source setting (AMPS) Recorder reading at direct output -1 x 10-10 1.0 MV +-2% -1 x 10-9 10.0 MV +-2% -1 x 10-8 0.100 V +-2% -1 x 10 1.0 V +-2% -7 -1 x 10-6 V +-2% 69 Appendix B: Manufacturer’s manuals 4. FPD Square Root Mode Test A. Set the Linear / Sq. Root Switch (SW3) to Square Root Mode B. Set diode oven temperature adjustment pot (R59) near the center of its range of adjustment. Monitor U3.6 with oscilloscope for oscillation or other signs of faulty circuit operation. C. Connect a variable span recorder or DVM (10 megoluns input impedance minimum) to the lOV output (CONl. 4), and a current source to the input connector (J3). Set the ZERO SW to ON. D. Check electrometer and recorder zeros and carefully rese t if necessary. Refer to Section 3, FPD Linear Mode Test, for zero set procedure. E. Set the ZERO SW to ON, the input current to -4.0 X 10·8 amps and adjust the diode oven temperature by means ofR59 so that when temperature stabilizes the recorder or DVM reads 31.56 mV as closely as possible. F. Reset input current to zero and note recorder/DVM reading. Return input current to-4.0 X 1·0 8 and trim diode oven temperature if necessary so that the difference in recorder/DVMreadings for input currents of zero and -4.0 X 10·8 amps is 31.56mV, plus or minus O. l mv. G. Check response curve per following table. (lf zero reading falls outside permitted limits, readjust the offset pot (R57) and repeat previous step. Current source setting (AMPS) 5. Direct output (10 VFS) reading (mV) -0.00 x 10-11 -0.5 ¸ “Zero” < +0.5 R62 = 191K R62 = 90.9K -2.00 x 10-11 “Zero reading” +.167 + .1 +.335 +-.1 -6.00 x 10-11 “Zero reading” +.470 + -.15 _.945+-1.5 -1.60 x 10-10 “Zero reading” +1.16 +-.2 +2.34+-.2 -6.40 x 10 “Zero reading” +3.34 + -.3 +6.71+-.3 -2.50 x 10-9 “Zero reading” +7.62 +-.6 +15.3 +-.6 -1.00 x 10-8 “Zero reading” +15.68 +-.9 +31.5+-.9 -4.00 x 10 -8 “Zero reading” +31.56 +-.1 +63.4 +-.1 -1.60 x 10-7 “Zero reading” +64.7 +-3.0 +130 +-3.0 -6.40 x 10-7 “Zero reading” +129 +-5.0 +260 +5.0 -2.56 x 10 “Zero reading” +319 +-12 +641 +-12 -10 -6 Noise and Drift Test A. Conduct test with all shields and covers in place and electrometer operating in the "square root" mode. (SW3 set to square root) Connect lOMV F.S. recorder to the Direct Output (CONl.4) with the chart speed set to approx. 0.25 cm/min. Disconnect input cable, tum the Zero Switch (SW4) ON and set the zero control pot (R38) so that trace is near center of plot. B. Record data for at least 30 minutes in a stable ambient temperature. C. Acceptance specifications are as follows: 70 1. Max. Peak-to-peak noise - 2% of full scale. 2. Occasional unexplained spikes - no more than one per half hour and not to exceed 5% full-scale peak height. 3. Max. Drift - 1.5% full scale during half hour nm. Appendix B: Manufacturer’s manuals 6. FPD Thermocouple Temperature Setup. The thermocouple input at CONS Pin1 and Pin2 will be factory adjusted to operate with Detector temperatures that range from approximately 150 Degrees C to 200 Degrees C. R e t u r n O i r e c t t o P o w e r S u p p l y ( G N D ) S W 1 8 L E D A 6 5 1 D V 4 1 V 3 S W C O M 71 Appendix B: Manufacturer’s manuals 72 Appendix B: Manufacturer’s manuals 73 Appendix B: Manufacturer’s manuals 74 Appendix B: Manufacturer’s manuals 75 Appendix B: Manufacturer’s manuals 76 Appendix B: Manufacturer’s manuals 77 Appendix B: Manufacturer’s manuals 78 Appendix B: Manufacturer’s manuals 79 Appendix B: Manufacturer’s manuals 80 Appendix B: Manufacturer’s manuals 81 Appendix B: Manufacturer’s manuals 82 Appendix B: Manufacturer’s manuals 83 Appendix B: Manufacturer’s manuals 84 Appendix B: Manufacturer’s manuals 85 Appendix B: Manufacturer’s manuals 86 Appendix B: Manufacturer’s manuals 87 Appendix B: Manufacturer’s manuals 88 Appendix B: Manufacturer’s manuals 89 Appendix B: Manufacturer’s manuals 90 Appendix B: Manufacturer’s manuals 91 Appendix B: Manufacturer’s manuals 92 Appendix B: Manufacturer’s manuals 93 Appendix B: Manufacturer’s manuals 94 Appendix B: Manufacturer’s manuals 95 Appendix B: Manufacturer’s manuals 96 Appendix B: Manufacturer’s manuals 97 Appendix B: Manufacturer’s manuals 98 Appendix B: Manufacturer’s manuals 99 Appendix B: Manufacturer’s manuals 100 Appendix B: Manufacturer’s manuals 101 Appendix B: Manufacturer’s manuals 102 Appendix B: Manufacturer’s manuals 103 Appendix B: Manufacturer’s manuals 104 Appendix B: Manufacturer’s manuals 105 Appendix B: Manufacturer’s manuals 106 Appendix C: Spare Parts List C Appendix C: Spare Parts List 02122 0020 Hydrogen shut-off valve (Alcon) 02122 0023 O-ring kit for Alcon valve 02122 0044 Hydrogen shut-off valve (Asco) 02122 0057 O-ring kit for Asco valve 4-5000-391 Utility gas regulator (H2 or air) 59551 2097 Heater (flame cell and exhaust breather) 116901-GUB Photometric tube 115000-0008 Power supply for electrometer board 115003-0001 Electrometer board 116910-KALREZ O-ring kit for flame cell and detector 116906-0001 Ignitor with Kalrez O-ring 23608-0019 Heat filter 23608-0027 Optical filter NOTICE For price & delivery information please contact your local Emerson Sales office, or email gc.csc@emerson.com. NOTICE For spare parts for Model 500 or Model 700 Gas Chromatographs, please refer to the appropriate GC manual. 107 109 FPD for Gas Chromatographs Manual 7R00370-H01 October 2017 North America Regional Office Emerson Automation Solutions 10241 West Little York, Suite 2200 Houston, TX 77040 USA +1 866 422 3683 or +1 713 396 8880 +1 713 468 8175 GC.CSC@Emerson.com Latin America Regional Office Emerson Automation Solutions 1300 Concord Terrace, Suite 400 Sunrise, FL 33323, USA +1 954 846 5030 +1 952846 5121 GC.CSC@Emerson.com Europe Regional Office Emerson Automation Solutions Europe GmbH Neuhofstrasse 19a P.O. Box 1046 CH 6340 Baar Switzerland +1 954 846 5030 +1 952846 5121 GC.CSC@Emerson.com Asia Pacific Regional Office Emerson Automation Solutions Asia Pacific Pte LTD 1 Pandan Crescent Singapore 128461 +65 6777 8211 +65 6777 0947 GC.CSC@Emerson.com Analyticexpert.com Linkedin.com/company/Emerson-Automation-Solutions Twitter.com/Rosemount_News Facebook.com/Rosemount Middle East and Africa Regional Office Emerson Automation Solutions Emerson FZE P.O. Box 17033 Jebel Ali Free Zone - South 2 +971 4 8118100 +971 4 88665465 GC.CSC@Emerson.com Youtube.com/user/RosemountMeasurement Google.com/+RosemountMeasurement The Emerson logo is a trademark and service mark of Emerson Electric Co. Rosemount and Rosemount logotype are trademarks of Emerson. All other marks are the property of their respective owners. © 2017 Emerson. All rights reserved.