Pickering Laboratories PCX 5200 Operation Manual Download

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Operation Manual

PCX 5200

Post-column

Derivatization Instrument

Pickering Laboratories, Inc.

1280 Space Park Way

Mountain View, CA 94043

(800) 654-3330

International: (650) 694-6700

Fax: (650) 968-0749

Website: http://www.pickeringlabs.com

E-mail: [email protected]

Cat. No. 0101-0001

Version 6, January 2002

KERIN

LAB

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Summary of Contents for PCX 5200

Page 1: ...Laboratories Inc 1280 Space Park Way Mountain View CA 94043 800 654 3330 International 650 694 6700 Fax 650 968 0749 Website http www pickeringlabs com E mail support pickeringlabs com Cat No 0101 0001 Version 6 January 2002 Pickering Laboratories Inc PICKERING LABORATORIE S ...

Page 2: ...PCX 5200 User s Manual Contents ...

Page 3: ...a Post column System 1 5 Chapter 2 PCX5200 System Components PCX5200 Post column Instrument 2 1 Getting to Know Your PCX5200 2 1 Front Panels 2 1 Internal 2 3 Rear Panel 2 4 Column Oven 2 6 Reagent Reservoirs 2 8 External Reagent Pressurization System 2 9 Keypad and Liquid Crystal Display User Interface 2 10 Keypad Examples 2 13 Loading a Preset 2 13 Saving a Preset 2 15 Flow Diagrams 2 18 PRESET ...

Page 4: ... 3 8 Piston wash System 3 8 Priming the Reagent Pump 3 9 System Testing Verification 3 9 Shutdown 3 10 Short term 3 10 Medium term 3 11 Long term 3 12 Chapter 4 Routine Maintenance Troubleshooting Initial System Testing 4 1 Test Chromatogram 4 1 Paramater Log 4 1 Precautions Problem Prevention 4 2 Mobile Phase 4 2 Back flow Prevention 4 2 Reactor Precautions 4 2 Electrical Precaution 4 2 Routine M...

Page 5: ...4 13 Interpretation of Pressures 4 14 Two reagent PCX5200 4 14 One reagent PCX5200 4 14 Cleaning the Post column System 4 15 Fittings 4 15 External 4 15 Internal 4 15 Internal Spill 4 15 Appendix A PCX5200 Parameter Log A 1 Analytical Conditions A 2 Post column Band spreading Test A 3 Appendix B Spare Parts B 1 References Limited Warranty Index ...

Page 6: ...s 2 3 and 3 8 about the piston wash system of the post column pump A note supplies supplementary information which may be helpful or necessary for better understanding of the material The caution calls attention to an operating procedure practice or the like which if not correctly done or adhered to could result in loss of information or damage to or destruction of part or all of the equipment Do ...

Page 7: ...t eine Gefahr Es macht aufmerksam auf einen Vorgang eine Handhabung oder ein Vorhaben die bei unkorrektem Befolgen der Vorschriften zu einer Verletzung oder einer lebensgefährlichen Situation führen können El signo de atención indica un riesgo Requiere atención sobre un procedimiento práctica o similar que si no se ejecuta correctamente o se sigue minuciosamente prodía producir heridas o muerte No...

Page 8: ...r durch hohe Temperaturen Es macht aufmerksam auf den Heizblock des Saulenofens der heißer als 70 C sein kann Zu Ihrer Sicherheit sollten Sie isolierende Handschuhe tragen wenn der Saulenofen warm ist Este signo de atención indica una superficie caliente un riesgo de alta temperatura Pide atención sobre un bloque calefactor de columnas por encima de 70 C Para su seguridad use guantes aislantes cua...

Page 9: ...r On En marche An Escendido Acceso Power Off Éteint Aus Apagado Spento Fuse Specification Spécification du fusible Spezifikation der Sicherung Fusible Valvole Specificazioni Protective Ground Prise de terre Erdung Masa de protección Protezioni a terra ...

Page 10: ...to give reliable results Stability of Reagent The minimum reagent stability sufficient for routine work is one day This means that the yield and signal to noise ratio for a given sample must remain constant for at least 8 hours Speed of Reaction The analytical separation is complete when the reagent is mixed with the column effluent Therefore in order to minimize band spreading it is important to ...

Page 11: ...hows the pump pressure for diagnostic purposes 2 It absorbs pulses by the spring action of the Bourdon tube There is a packed bed restrictor just downstream to provide a load for the pressure gauge so that it will effectively absorb pulsations Referring to Fig 1 1 the anti siphon valve prevents the gas pressure in the reservoir from forcing liquid through the system with the power off The post col...

Page 12: ...or Pre column Filter 0 5µm Thermostatted Column and Guard Heated Reactor Detector Back pressure Regulator 100 psi Waste 500 psi Pressure Switch Over pressure relief valve 525 psi Waste 2 1 3 Post column Pump Reagent Pressure Bypass Valves Reagent Filters 2µm Restrictors Anti siphon Valves 40 psi Post column Pressure Pressurized Reagent Bottles LC Eluants LC Pump Injector Pre column Filter 0 5µm Th...

Page 13: ...ector with nothing in between the baseline from the detector shows a periodic noise Figure 1 2 the time period is equivalent to the pump stroke The Elements of an HPLC with Post column Sytem Design of an HPLC Figure 1 2 Now add a commercial pulse damper The baseline is still not smooth the periodic noise is still there although less pronounced Figure 1 3 Figure 1 3 Eluants LC Pump Injector Detecto...

Page 14: ...tant flow we need to add a reservoir pulse damper and a dam column The flow downstream from the dam is constant smooth baseline What happens if we simply add a post column pump a mixing tee and a reactor What happens to the baseline The periodic noise returns created by the post column pump Figure 1 5 Designing a Post column System Figure 1 4 Figure 1 5 Pulse Damper Eluants LC Pump Injector Pre co...

Page 15: ...gent Just follow the same procedure Another post column pump pressure gauge restrictor mixing tee and reactor We add a post column pressure gauge Fig 1 1 to determine if there is any blockages in the reactors Note that the pressure in the post column gauge is stable because it is down stream from the analytical column and the restrictors i e standing down stream from the reservoir and dam in our e...

Page 16: ... Instrument Getting to Know Your PCX5200 Front Panels On the post column panel the post column pressure gauge measures the liquid pressure at the first mixing tee This is effectively the pressure on the heated reactor ambient reactor and dectector This gauge indicates pressure when liquid is flowing through the system The liquid connections to the pressure sensor are labelled From LC Pump and To I...

Page 17: ...olumn Derivatizer TO INJECTOR FROM PUMP FROM INJECTOR TO DETECTOR OVER PRESSURE RELIEF POST COLUMN PRESSURE REAGENT 1 PRESSURE BYPASS 1 REAGENT 2 PRESSURE BYPASS 2 600 400 200 800 1000 500 PCX 5200 REAGENT 1 PRES STATUS COLUMN TEMP PUMP ENABLE POWER REACTOR TEMP PROG REAGENT 2 PRE SET PICKERING LABORATORIES Model PCX 5200 Post Column Derivatizer TO INJECTOR FROM PUMP FROM INJECTOR TO DETECTOR OVER...

Page 18: ...the Reagent 2 pressure gauge operates the same as the Reagent 1 pressure gauge The Bypass 2 valve is used to purge and prime the second reagent pump and it operates the same as the Bypass 1 valve The three removable front panels gives access to the liquid ends of the pump reagent filters restrictors the thermostatted reactor electrical connections for the reagent pump and the flow adjustment knobs...

Page 19: ...our local reseller may have provided the correct local cord set If your local power outlets are different you will need to obtain the appropriate grounded cord set The main power switch is located in the power connector assembly The fuse holder is located in the power connector assembly To change the fuse first remove the power cord from the connector Carefully pry out the fuse clip with a small s...

Page 20: ... Cuidado Asegúrese que el cable de red está desconectado antes de instalar o cambiar un fusible Attenzione Assicuratevi che il cavo di alimentazione sia scollegato prima di installare o sostituire un fusible Waarschuwing Zorg dat de voedingskabel losgekoppeld is voordat een zekering wordt geplaatst of vervangen Avvertimento Fare atenzione che la corda del voltaggio sia staccata prima di cambiare v...

Page 21: ...ytical and guard column The heater block is slotted to receive the analytical column 5 10 15 and 25 cm long The last part of the lead in capillary is embedded in the heating block to preheat the eluant for a more uniform temperature within the column The lead in capillary is 0 007 inch 0 17 mm ID to minimize loss of efficiency Figure 2 6 Column Guard column Column Oven ...

Page 22: ...lorsque le four de la colonne est chaud Warnung Der Heizblock des Säulenofens könnte heißer als 70 C werden Für Ihre Sicherheit sollten Sie isolierende Handschuhe tragen wenn der Säulenofen warm ist Atención El bloque calefactor de columnas puede estar por encima de 70 C Para su seguridad use guantes aislantes cuando el horno de columnas esté caliente Avvertimento Il blocco della colonna potrá div...

Page 23: ...Atención Para su seguridad las botellas están recubiertas con una resistente película plástica y están constrastadas a 15 psig 1 bar No utilice botellas sin recubrimiento Avvertimento Per la sua protezione le bottiglie sono construite forti con un percentuale du plastica e sono usabili per un massimo di una Bar 15 psi Non usare bottiglie normali The Gas Inlet fitting is where inert gas enters the ...

Page 24: ...nt bottle cap directly facing the shut off valve Connect the Trione ninhydrin or OPA reagent to the Saran tubing and connect the Hydrolysis or Oxidizing reagent to the Teflon tubing Nuts and reversed ferrules 1 4 28 are provided The reservoir cap has a built in vent valve The large white knob is the valve pull it up for CLOSED and push it down for OPEN If the gas is turned on opening the vent valv...

Page 25: ... To reach the advanced options menus hold a function key and press the PROG key The following table summarizes the keypad behavior POWER indicator light LED is useful as an indicator that the PCX5200 is connected to a power source and the on off switch on the back of the PCX5200 is turned on Keypad and Liquid Crystal Display User Interface Key ENABLE PUMP STATUS COLUMN TEMP COLUMN PRES REACTOR TEM...

Page 26: ... oven To change the setpoint press and hold the COLUMN TEMP key and press the key to increase or press the key to decrease Pressing the REACTOR TEMP key shows the process temperature of the reactor to the nearest degree and one of the three signs and indicating that the process temperature is less than equal to or greater than the set temperature respectively A flashing indicates the reactor is he...

Page 27: ...LC column pressure is at least 500 psi 34 bar ii The ENABLE key has been pressed 3 PUMP LED is green when two conditions are fulfilled i The PCX5200 is enabled ii The PUMP key has been pressed 4 STATUS LED turns orange when the PCX5200 is enabled but the set temperatures are not ready or the post column pump is off The STATUS LED turns green when the set temperatures are ready and the post column ...

Page 28: ... PRESET key each time will change to the next preset program Of course by pressing the key instead of the key you could go back to the previous preset program These 3a d steps are optional but it will help you to familiarize with other functions 3a Press the column TEMP key the LCD displays the current temperature of the column oven Column C The sign indicates that the temperature of the column ov...

Page 29: ...ess and hold the COLUMN PRES key While holding the COLUMN PRES key press the PROG key the LCD displays the maximum pressure Pres Max 260 bar the PROG LED turns orange To change the maximum pressure press and hold the PROG key While holding the PROG key press the or key to change the pressure we do not recommend any changes Press the key the LCD displays the minimum pressure Pres Min 32 bar To chan...

Page 30: ...t us review the parameters 1 Column oven 55 C 2 Column oven remains on at all time i e not slaved to the pressure interlock 3 Heated reactor 36 C 4 Save as Preset program 5 and title it Na AA OPA 1 To adjust the set temperature of the column oven press and hold the COLUMN TEMP key and then press the or key to obtain a readout of Column set 55 C 2 Next we want to set up the column oven to warm up a...

Page 31: ...te that program 5 may or may not have a name assigned to it yet If it is already in use the LCD would show 5 S name of program If that is the case press the or key until the LCD shows just S If all five preset programs are filled you need to write over one of them If you do not want to override any of the five preset programs press the key until the LCD shows Back YES and press the PROG key to exi...

Page 32: ... 2 2 17 Press the PROG key to accept the LCD shows Save Preset Press the key three times the LCD changes to Preset Name Erase Preset and then Back YES Press the PROG key to accept the LCD shows 5 Na AA Program number 5 is now ready ...

Page 33: ...N Interlock OFF Interlock ON Int reset Prop band Cycle sec Deriv Deriv App Back YES NO C Span C Offset Back YES NO Back YES NO Save Changes NO YES C PID C RTD Set Interlock PROG TEMP COLUMN PRE SET Preset 1 Name 2 Name 3 Name 4 Name 5 Name For all of the diagrams below press and hold the function key i e PRESET TEMP then press or PROG For PROG functions release the keys when the PROG LED turns ora...

Page 34: ...k YES NO R PID R RTD Interlocked PROG TEMP REACTOR 1 N name 1 2 N name 2 3 N name 3 4 N name 4 5 N name 5 Save Preset Preset Name Erase Preset Back YES 1 S name 1 2 S name 2 3 S name 3 4 S name 4 5 S name 5 1 N name 1 2 N name 2 3 N name 3 4 N name 4 5 N name 5 Back YES 1 E name 1 2 E name 2 3 E name 3 4 E name 4 5 E name 5 Back YES PROG PRE SET ...

Page 35: ...glass Sapphire UHMW polyethylene Dimensions 37 cm x 38 cm x 38 cm h x w x d Weight 13 to 15 kg depending on configuration Electrical Power 100 120 V 50 60 Hz 1 7 A 200 W grounded supply or 200 240 V 50 60 Hz 0 8 A 200 W grounded supply Installation overvoltage category II Pollution degree 2 Environmental Indoor use only Altitude up to 2 000 m 6500 ft Ambient temperature 5 40 C 40 104 F Relative hu...

Page 36: ...PCX5200 Instructions for how to do this will accompany the firmware package We need your comments to support the firmware If you discover a bug report it in writing to our Customer Service Department We will also consider your written suggestions for new features or other enhancements This device complies with Part 15 Class A of the FCC Rules Operation is subject to the following two conditions 1 ...

Page 37: ...PCX5200 User s Manual Chapter 2 2 22 ...

Page 38: ...ust be capable of binary gradient elution For amino acids or ALKION column applications the HPLC pump must be capable of ternary gradient elution HPLC manual injector or autosampler The injector should be able to inject a 10 µL sample preferably by full loop injection If drinking water is to be analyzed for carbamate insecticide residues the injector should be able to inject at least 200 µL and pr...

Page 39: ...rchased the user will need to provide adequate lengths of capillary tubing to connect HPLC pump and injector to pressure sensor 0 010 0 020 inch ID to detector inlet 0 010 inch ID to detector outlet 0 010 0 020 inch ID and to injector outlet 0 007 0 010 inch ID The user also needs to check the chemistry requirement for the specific application Placement of the LC system and detector can be on eith...

Page 40: ...tal compression fittings be careful not to over tighten as the tubing can collapse or crack Turn on the main gas supply Switch the toggle valve to the ON position to start gas flow Let the gas system purge for about one minute Switch the toggle valve down to OFF 2 Using the 0 5m Saran tubing PN 2103 0463 connect the reservoir to the gas outlet manifold There are three fittings on each bottle cap t...

Page 41: ...nect the pressure sensor to the inlet of the injector or autosampler Use the fitting labelled To Injector 2 Alternate method for amino acid analysis with mobile phases with pH 3 to minimize corrosion of the sensor or some integrated HPLC systems to minimize tubing runs Use two pieces of 1 16 inch x 0 020 inch ID capillary tubing to connect a tee fitting between the outlet of the HPLC pump and the ...

Page 42: ...SS 1 REAGENT 2 PRESSURE BYPASS 2 LC Pump Injector 2000 1000 500 2500 3000 1500 600 400 200 800 1000 500 2000 1000 500 2500 3000 1500 PCX 5200 REAGENT 1 PRES STATUS COLUMN TEMP PUMP ENABLE POWER REACTOR TEMP PROG REAGENT 2 PRE SET PICKERING LABORATORIES Model PCX 5200 Post Column Derivatizer TO INJECTOR FROM PUMP FROM INJECTOR TO DETECTOR OVER PRESSURE RELIEF POST COLUMN PRESSURE REAGENT 1 PRESSURE...

Page 43: ...ID inlet tubing red and heat exchanger from the left side of the detector to the flowcell behind the front panel of the detector with a 0 25 mm ID tubing HP Cat No 79881 67302 or Pickering Cat No 3110 6045 blue tubing to reduce the back pressure 3 Connect a 1 16 inch x 0 020 inch ID tubing from the outlet of the flowcell to the external 100psi backpressure regulator using a 1 4 28 nut with a 1 16 ...

Page 44: ...f the analytical column 4 Loosely fit the inlet of the guard column to the eluant heat exchanger Carefully lay the analytical column into its slot in the heating block 5 Turn on the HPLC pump at 0 2 ml min at 100 of the column storage solution 6 Wait for liquid to drip from the heat exchanger Tighten the connection to the guard Wait for liquid to drip from the inlet of the column and then tighten ...

Page 45: ...he piston seal wash system on your HPLC so that you can flush them at the same time The piston wash system is designed to flush the back end of the primary seal which significantly extends seal life However if a pump with a piston wash system is used without liquid in the piston wash system the secondary seal will wear out quickly because it is dry It can then scratch the piston and the scratched ...

Page 46: ... no bubbles come through 6 Close the valve remove the syringe and wash the Luer fitting with a little water 7 Repeat the process for the other valve if applicable If priming the reagent pump is difficult see Chapter 4 p 4 13 Read the Application Manual if applicable to become familiar with the use of your instrument In Chapter 4 of this manual there are procedures for the initial system testing Th...

Page 47: ...e PCX5200 either manually by pressing the ENABLE key or via the Slowdown program see below 2 Set the HPLC pump at the normal flow rate to flush the system for at least 20 minutes to allow the heated reactor to cool Choose an eluant that elutes contaminants from the column for example methanol for a reversed phase column and regenerant for an ion exchange column 3 Set the HPLC pump to 0 1 mL min 4 ...

Page 48: ...in the reagent reservoir with water methanol approximately 1 1 5 Turn off the fluorescence detector and HPLC pump 7 Loosen the fitting at the inlet of the 100 psi external back pressure regulator relieving pressure on the post column system Place paper towels under the back pressure regulator to absorb any escaping liquid 8 Relieve the pressure in the reagent gauges by briefly opening the bypass v...

Page 49: ...water 7 Increase the flow rate of the HPLC to give 500 psi on the post column system 8 Flush the entire system for 30 minutes then replace the water on the HPLC with 80 20 water methanol 9 Replace the water in the reagent reservoir with water methanol 80 20 10 Start the HPLC and reagents pumps and flush the system for another 10 minutes 11 Relieve the pressure in the reagent gauge s by briefly ope...

Page 50: ...milar log from factory testing Use the same conditions as for the test chromatogram above Report the pressures for the system equilibrated under initial conditions The pressures reported for Reagent 1 and Reagent 2 should be the maximum swings of the pointers Although the parameters will not be identical to the factory they should be similar Keep a daily log of the four pressures for diagnostic us...

Page 51: ...t pump can be engaged The second is a pair of automatic valves that prevent gas pressure from pumping reagents back through the column during extended shutdowns However there are ways that the safety systems can be bypassed accidentally For example residual pressure in the gauges immediately after shutdown will take some time to leak down to zero Follow these procedures to avoid such accidents Nev...

Page 52: ...tion replace the piston seal You will need to purchase a seal kit 3106 1310 including two seals two back up washers a 5 32 hex wrench and a seal installation tool Extra seals and a preventive maintenance kit may also be ordered from Pickering Laboratories see Appendix B Additional tools needed for piston seal change are 1 4 and 1 2 open end wrench Open end wrenches can be purchased at local hardwa...

Page 53: ...washer and piston seal Discard the seal The back up washer is usually reusable Do not scratch the walls of the seal cavity with the tool 9 Inspect the retainer Clean the retainer if necessary If there is evidence of wear or the piston does not fit snugly in the retainer or the retainer grips the piston too tightly the retainer should be replaced 10 This step is only necessary if there are signs of...

Page 54: ...d and wash system as shown in Figure 4 1 Hold the pump assembly firmly in place and reinstall it on the pump in line with the axis of the piston do not tilt the pump head sideways 14 If the post column pump is a duplex pump repeat steps 6 13 for reagent 2 side 15 Replace the pump tighten the captive screw and reconnect the electrical connection 16 Reconnect the tubings to the pump head stabilize t...

Page 55: ...he reagent inlet line from the bottom of the pump head Wipe up any spilled liquid Disconnect the outlet tubing from the top of the pump head stabilize the outlet check valve with a 1 2 wrench when removing the 1 16 fitting to prevent the check valve from moving 4 Remove the pump from the chassis by loosening the captive screw and unplugging the electrical connector Place the pump in a more accessi...

Page 56: ...the outlet check valve Remove the check valves with a 1 2 wrench counter clockwise After removal keep the valve oriented so the translucent washer faces upwards 1 Remove plastic cover 2 Insert the new inlet check valve into the pump head and tighten by hand until just finger tight Tighten with a 1 2 wrench 1 8 to 1 4 turn more Do not overtighten The sapphire seats may crack 3 Turn the pump head up...

Page 57: ... the larger dowel pin 3 16 od Make sure that the valve insert is oriented correctly 4 Press a new Kel F valve seal into the valve housing 5 Slide the check valve cartridge into the valve housing making certain the cartridge is oriented correctly 6 Press a second valve seal into the valve housing This valve seal will extend approximately 0 02 0 03 from the valve housing Rebuilding Check valves Figu...

Page 58: ... It is superficially similar to the 2 µm reagent filter so take care not to confuse them 4 Replace the filter element Tighten the filter element firmly 5 Reconnect the capillary tubing Pre column Filter 2000 1000 500 2500 3000 1500 600 400 200 800 1000 500 2000 1000 500 2500 3000 1500 PCX 5200 REAGENT 1 PRES STATUS COLUMN TEMP PUMP ENABLE POWER REACTOR TEMP PROG REAGENT 2 PRE SET PICKERING LABORAT...

Page 59: ...e detached flow conditioner panel in a more accessible place to continue Repeat the same procedures for the second flow conditioner panel 4 Disconnect the tubings from the filter Use a 7 16 inch wrench and a 9 16 inch wrench to disassemble the filter 5 Replace the filter element The correct filter element is 3102 9040 a 2 µm frit It is superficially similar to the pre column 0 5 µm filter so take ...

Page 60: ...ydrindantin from expired Trione ninhydrin solution Please read the troubleshooting section in the Application Manual for some easy fixes Generally chemical clogging problems can be solved with chemistry Changing the heated or ambient reactor is your last resort after attempts to clean the reactor have failed 1 Shutdown the post column system and let the reactor cool for at least 30 min 2 Remove th...

Page 61: ...firm the problem before fixing it Substitution Rule Swap in a good part for a questionable one Put it Back If swapping does not fix it put the original back in Write it Down Changes or modifications incidents Crystal Ball Preventive maintenance saves more time in the long run Buffer Rule Remove buffers from LC when not in use General Procedure for Troubleshooting Examine the system front to back R...

Page 62: ... on or off it makes little difference 2 Connect the 20 mL priming syringe to the bypass Open the Bypass valve Draw liquid until no bubbles come through Empty the syringe and reconnect it to the bypass 3 Close the liquid shut off valve on top of the post column reagent reservoir 4 Pull a vacuum with the syringe Hold the vacuum until no more bubbles come out This causes the trapped bubbles to expand...

Page 63: ...essures specific to your system Condition Column Post Column Reagent 1 Reagent 2 Normal 1200 250 1500 1500 Pre column filter blocked Heated reactor obstructed Ambient reactor obstructed Reagent 1 not pumping Reagent 2 not pumping Restrictor 1 blocked Restrictor 2 blocked Condition Column Post Column Reagent Normal 1200 250 1500 Pre column filter blocked Reactor obstructed Reagent not pumping Restr...

Page 64: ...nge Clean spill area with a wet towel and thoroughly dry Do not spray water directly into the instrument Vacuum clean inside the post column system once a year 1 Open the column oven door 2 The reagent flow conditioners can be removed by removing two captive screws Set the flow conditioners upside down in the front of the column oven You do not need to disconnect any tubings 3 The post column pane...

Page 65: ...PCX5200 User s Manual Chapter 4 4 16 ...

Page 66: ...low Rate Medium Pump 2 Micrometer Flow Rate Medium Normal Pressures and Flows at Initial Conditions Flow Rate Pressure Analytical Pump Reagent Pump 1 Reagent Pump 2 Post Column Temperature Analytical Column Heated Reactor Room Tested by Date PCX 5200 Parameter Log ...

Page 67: ...Rate Gradient Program Column Type ID Temperature Injector Autosampler Sample Volume Solvent Manual Auto Other Parameters Detector Excitation Band Emission Band Range PMT Lamp Resp time Integrator or Data Station Range or Scale Units Attenuation Chart Speed Peak Threshold Width Run Time Operator Date Reference ...

Page 68: ... Excitation Emission Lamp PMT gain Range Attn Integrator Range Attn Units Multiplier Chart speed Method for calculating peak width Part 1 Column connected directly to the detector Post column pumps off reactor temperature 55 C Run Retention time Peak width Average Wd Part 2 Post column reactors connected to column and detector Post column pumps off normal reactor temperature Run Retention time Pea...

Page 69: ...column delay volume is about 600 µL The delay time can be calculated as t 0 5 fe fR1 0 1 fe fR1 fR2 where fe is eluant flow rate fR1 is first reagent flow rate and fR2 is second reagent flow rate 0 5 is the volume of the first reactor and 0 1 is the volume of the second ...

Page 70: ...p with piston washing system 3106 1322 Piston Guide Retainer 3106 1324 Liquid End Assembly 3107 0137 Reagent bottle coated 1 liter borosilicate with cap for storage 3107 0300 Reagent bottle assembly cap with integrated 2 way valve 2103 0463 Tubing Saran 1 8 OD x 0 063 ID per 3 ft 90 cm 3104 0081 Seal Kit for bypass valve 3101 0060 Nut Fingertight for 1 16 plastic tubing 3102 1202 Nut male Upchurch...

Page 71: ...ith post column fluorescence derivatization Anal Chem 56 1984 2465 2475 H Frister H Meisel and E Schlimme OPA Method Modified by Use of N N Dimethyl 2 mercaptoethylammonium Chloride Fresenius Z Anal Chem 330 1988 631 633 Glyphosate J E Cowell Analytical Residue Method for N Phosphono methylglycine and Aminomethylphosponic acid in Environmental Water Monsanto Method Number 86 63 1 1987 Environmenta...

Page 72: ...nalysis D H Spackman W H Stein and S Moore Anal Chem 30 1958 1190 M V Pickering LC GC 7 1988 484 J A Grunau and J M Swiader J Chromatogr 594 1992 165 A A Boulton G B Baker and J D Wood Eds Neuromethods 3 Amino Acids Humana Press Clifton NJ 1985 Chapter 1 ...

Page 73: ...ring will replace the Analytical Column under warranty if found defective in material or workmanship However the warranty is void if the Analytical Column was damaged due to Customer s misuse Ion Exchange columns for Amino Acid Analysis Glyphosate and ALKION columns are warranted for 90 days Silica based reversed phase columns are warranted for 30 days How to Obtain Warranty Service If there is a ...

Page 74: ......

Page 75: ...t column system 1 5 Detector 3 1 Detector connections 3 6 Downloading firmware 2 21 E Electrical precaution 4 2 Electrical requirement 3 2 ENABLE key 2 10 F Filter pre column 4 9 Filter reagent 4 10 Fittings 3 3 Flow diagrams 2 18 Flow conditioner 1 6 2 3 Flow conditioner panel 2 1 Front panels 2 1 Fuse 4 12 Fuse 2 4 G Gas pressure system 2 9 Gas regulator 2 9 Gauge 1 2 Guard 3 7 H Heated reactor ...

Page 76: ...Radio frequency 2 21 Reactor precautions 4 2 Reagent filter 4 10 Reagent pump 3 8 Reagent reservoir 2 8 3 3 Rebuilding check valves 4 8 Removing check valves 4 7 Reservoir 3 3 Reversed ferrule 3 3 Reagent pump 4 3 Rotor seal 3 1 Routine maintenance 4 3 RS232 2 4 2 21 S Saran tubing 3 3 Saving a Preset program 2 15 Seal replacemen reagent pump 4 3 Shutdown 3 10 Slowdown program 3 10 Space requireme...

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