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Section 4. Operating the Electrochemical Detector

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Summary of Contents for LC-4C

Page 1: ...derutilized and idle equipment along with credit for buybacks and trade ins Custom engineering so your equipment works exactly as you specify Critical and expedited services Leasing Rentals Demos In s...

Page 2: ...MANUAL Electrochemical Detector B i o a n a l y t i c a l S y s t e m s I n c 2701 Kent Avenue W e s t L a f a y e t t e I n d i a n a 4 7 9 0 6 Artisan Technology Group Quality Instrumentation Guaran...

Page 3: ...ent Avenue West Lafayette IN USA 47906 1382 Phone 765 463 4527 Fax 765 497 1102 Never touch the electrochemical cell the cell wires or any part of the cell while the detector is operating Before touch...

Page 4: ...y Connections 15 Section 4 Operating the Electrochemical Detector 23 4 1 LC 4C Front Panel 23 4 2 LC 4C Rear Panel 27 4 3 CC 5 Rear Panel 31 4 4 Routine Operating Procedure 32 Section 5 Upgrading to a...

Page 5: ...Table of Contents ii Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Page 6: ...etween column and detector The LC 4C is a component of the LC 44 detector and the modular BAS 480 series of liquid chroma tographs The information in this manual represents the combined experience of...

Page 7: ...e CC 5 compart ment A removable panel on the back of the instrument is replaced by the LC 23C heat ing block which holds up to 2 cartridges This option is described in a separate man ual and product b...

Page 8: ...stems re fuses all unauthorized return shipments 2 3 Product Warranty BAS products are fully warranted against defects in material and workmanship The LC 4C amperometric controller is unconditionally...

Page 9: ...URN ANY PRODUCTS FOR SERVICE UNTIL A RETURN AUTHORIZATION NUMBER RA HAS BEEN OBTAINED The RA identifies you as the sender and describes the problem you are having in full detail Turnaround time on ser...

Page 10: ...s kets and reference electrode assembly Please retain the shipping box and packing material until you have fully tested the unit to be certain that no damage was incurred during shipping If there are...

Page 11: ...Electrode Jumper use is optional packaged with the electrode gaskets 17 PTFE Inlet Tubing 0 25 mm i d not shown packaged with detector accessories not used with cell preheater 18 20 L Loop not provide...

Page 12: ...S BAS 480 ANALYZER MADE IN USA CAUTION TO PREVENT ELECTRICAL SHOCK DO NOT REMOVE COVER NO USER SERVICEABLE PARTS INSIDE REFER SERVICING TO FACTORY PERSONNEL CONNECT ONLY TO LC 23C PROBE ON BAS LC 22C...

Page 13: ...ETPOINT HEATER 1 SETPOINT HEATER 2 DISPLAY SELECT DISPLAY UP DN POWER FILTER POTENTIAL MANUAL OFFSET _ RANGE _ OFF _ _ 100 10 1000 ON ZERO OFF ON TEST STBY AUTO ZERO MARKER CELL POWER 6 1 2 3 40 30 20...

Page 14: ...line cord and slide the plastic window to the left as shown in Figure 3 5 The orientation of the small circuit board now exposed in this socket determines the voltage option If the voltage labeled on...

Page 15: ...ontroller etc to the same grounded power line This ensures adequate ground to all components of the system and eliminates the possibility of a ground loop which could produce base line noise Also sele...

Page 16: ...llent flow rate precision and minimal pump pulsation The PM 80 Pump may be connected di rectly to the injection valve port see 26 in Figure 3 1 The PM 80 pump includes a pulse damper to reduce short t...

Page 17: ...plugs con nects to the corresponding set of banana jacks If you plugged the power cable into the HEATER1 connector plug the banana plugs into the PROBE1 jacks If you used HEATER2 for the power cord c...

Page 18: ...VER NO USER SERVICEABLE PARTS INSIDE REFER SERVICING TO FACTORY PERSONNEL CONNECT ONLY TO LC 23C PROBE ON BAS LC 22C CONNECT ONLY TO HEATER OUTLET ON BAS LC 22C 1V GND 10mV OXD RDN REMOTE CELL REZERO...

Page 19: ...ta system does not have a ground connect a wire included part 32 Figure 3 1 from the OUTPUT GND of the terminal strip to the threaded hole at the upper left corner of the rear panel If this is a dual...

Page 20: ...L of acetonitrile water 40 60 v v and divert all column ef fluent to a waste receptacle This flushing step cleans any chemicals remaining from previous injections from the column and also wets the hyd...

Page 21: ...ate e g 0 5 mL min and make connections to the flow cell as described in 6 or 7 below Place a lab tissue in the vicinity of the cell to help soak up the leakage while you complete attachments We recom...

Page 22: ...ment Note that the large side slots allow access for the column body even with the top down NOTE For units with cell temperature control preheater DO NOT allow the thin met al tubing on the inlet to t...

Page 23: ...hick TG 15M 0 015 381 m thick TG 2M 0 002 51 m thick Dead volume de termines how FAST the sample flows through the cell Changing gaskets allows you to influence this rate of flow independently of the...

Page 24: ...proceeding NOTE Removal and reinsertion of the reference electrode as in steps 10 12 is a useful technique to remove bubbles that have formed in the reference well Such bubbles produce a regular patt...

Page 25: ...al working electrode you may use either sensor and reserve the remaining one as a backup If using one as a generator electrode it must be up stream of the detector electrode Before connecting or disco...

Page 26: ...abel to working electrode 1 Black wire with W2 label to working electrode 2 The red and white wires are connected as for single electrode detectors see step 14 In most cases the generator electrode le...

Page 27: ...ve from W1 detector white lead red plug or HI recorder input black lead black plug or LO recorder input black jumper green plug recorder ground terminal LO is thus jumpered to GND from W2 detector whi...

Page 28: ...in V output current Output in nA or A auto offset current OffsetA in nA or A and manual offset current OffsetM in nA are chosen by pressing the up or down DISPLAY keys until the desired function is d...

Page 29: ...red voltage 0 1 900 V is displayed WORKING ELECTRODE POTENTIAL Any applied potential between 0 and 1 999 V can be selected by keying the DISPLAY to read App E then turning the POTENTIAL knob until the...

Page 30: ...ange chosen The range and sign of the offset are determined by two toggle switches located above the adjusting knob When set on the circuit will null anodic oxidative currents on it will null cathodic...

Page 31: ...0 02 Hz provides the greatest amount of filtering and 1 0 Hz provides the least amount If you wish to optimize the filter setting for your separation try several runs with different fil ter settings...

Page 32: ...rs and computer workstations Chart recorders can usually take negative going signals when using two detectors you may reverse one of the switches to have the pens coming from different sides of the ch...

Page 33: ...tential with an external volt meter and may be used in the self test procedure see Appendix I page 41 GEN This section of the terminal strip concerns the generator electrode The IGEN connector provide...

Page 34: ...UP DN 0 1 Afs UP DN DN UP DN 0 2 Afs DN UP DN UP DN 0 5 Afs UP UP DN UP DN 1 0 Afs DN DN UP UP DN 2 0 Afs UP DN UP UP DN 5 0 Afs DN UP UP UP DN 10 Afs UP UP UP UP DN 20 Afs DN DN DN DN UP 50 Afs UP D...

Page 35: ...UP UP DN DN 1 00 Hz DN UP DN DN Switch positions M N and O select the PC REMOTE selection see table below These set tings will allow up to 8 detectors to be independently addressed by a remote comput...

Page 36: ...Preheater Power switch see Figure 3 1 and Section 6 attenuates the wattage entering the preheater to about 60 in the Low setting The High setting transmits full AC power to the heater 10 W Selection...

Page 37: ...ccordingly 3 Zero the recorder with its zero control Baseline should be on the right side of the paper This may vary among chart recorder models 4 Turn the CELL switch to STBY 5 Turn the POWER switch...

Page 38: ...s that promote bacterial growth acetates citrates phosphates should not be recycled and should be changed every few days generally every two days Pump these at low flow rates when the system is not in...

Page 39: ...Section 4 Operating the Electrochemical Detector 34 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Page 40: ...panel 5 Set the detector components as shown in Figure 3 7 6 The cell lead cable terminates in two connectors that plug into the two LC 4Cs see Figure 5 1 The short larger diameter cable serves W1 and...

Page 41: ...rate W1 must be active first You may elect to operate W1 by itself as you would with a single LC 4C That is permissible the second LC 4C need not be powered The reverse mode is not possible however Fi...

Page 42: ...in the detector baseline In these cases both a column heater and a cell preheater may be needed In Figure 6 1 are shown plots of EC detector background current versus temperature The slope of the cur...

Page 43: ...drops The concentration gradient at the electrode surface is accentuated and the end effect is larger peak currents Taken separately the trends in both background current and peak current versus tempe...

Page 44: ...ation of Detector Preheater Module on CC 5 1 Open the CC 5 cover to the vertical position Remove the temporary cover from the rear panel 3 screws 2 Disconnect the tubing between the column and the det...

Page 45: ...plugs into the color matched jacks on the LC 22C Temperature Controller labeled PROBE 1 or PROBE 2 b Plug the Preheater Module power cord into the corresponding power receptacle HEATER 1 or HEATER 2 o...

Page 46: ...knob Readings on the voltmeter and the front panel display should be within 5 mV 8 Move the red probe of the voltmeter to the green 1 V output jack or the 1 V connector in the OUTPUT section of the t...

Page 47: ...turn to a POTENTIAL of 1 0 V and RANGE of 20 nA The OUTPUT should be 0 485 to 0 515 V Flip the rear panel switch to RDN The OUTPUT should now be 0 485 to 0 515 V Flip back to OXD 10 Flip the MANUAL OF...

Page 48: ...int for best performance and for the clamp circuit to operate If a strip chart recorder is connected to the LC 4CE a jumper wire between the or LO recorder input and recorder ground will provide the E...

Page 49: ...V NOTE The waveform is symmetrical around 0 V so if the positive amplitude is set to 1 00 V the negative portion of the waveform will be 1 00 V The other two controls are located on the bottom cover o...

Page 50: ...cell This switch uses 15 of the 16 available positions Position 0 marked as not used will disable the waveform generator NOTE The time is determined by counting the pulses at the set frequency so the...

Page 51: ...Appendix II Operation of the LC 4CE 46 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Page 52: ...mark front panel 25 remote 28 Column flushing 15 heater 2 Connections chromatography 15 electrical 12 20 40 Controls 23 D Damaged shipments 3 Default settings filter 30 gain range generator electrode...

Page 53: ...23 Fuse 9 G Gain range default setting 29 setting 24 Gaskets thin layer 18 Generator electrode GEN connections 12 20 28 default gain range 29 monitoring 28 29 setting 24 Grounding all components in s...

Page 54: ...tting working electrode 24 Power requirements 9 Power switch 23 Preheater connections 12 17 installation 17 39 setting 31 short circuit test 17 Pulse damper 11 Pump 11 R Range gain default setting 29...

Page 55: ...rage 33 T Temperature control 37 Terminal strip 28 Troubleshooting self test 41 short circuit test preheater 17 U Upgrades cable installation 35 dual detectors 35 preheater installation 39 V Voltage s...

Page 56: ...uipment Have surplus equipment taking up shelf space We ll give it a new home Learn more Visit us at artisantg com for more info on price quotes drivers technical specifications manuals and documentat...

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