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Antec Scientific ROXY Exceed Скачать руководство пользователя страница 67

Chapter 5

Measurement modes

67

Fig. 24. Potential steps in pulse mode. During t1 the measurement poten-
tial is applied, the actual current measurement occurs during ts. Steps t2,
t3 and t4 are for regenerating the electrode. This process repeats itself
continuously as soon as the cell is on.

In pulse mode up to five potential steps can be defined. The sampling in-
terval (period at which the current is measured) is applied at the end of E1.

Pulse mode - 2

In the ROXY Exceed an extended pulse mode, pulse mode - 2, is available
when operating the instrument via a PC using Dialogue Elite or Chro-
meleon CDS software. The pulse mode - 2 is not available in manual oper-
ation using keyboard/display. In the extended pulse mode it is possible to
program a multi-step waveform, with up to 30 time, potential (t,E) coordi-
nates, see figure below. Furthermore, the measurement time interval in
which the current is measured,

marked by a ‘Begin’ and ‘End’ marker, is

free programmable in the pulse table.

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Содержание ROXY Exceed

Страница 1: ...T 31 71 5813333 info AntecScientific com www AntecScientific com Antec Scientific Industrieweg 12 2382 NV Zoeterwoude The Netherlands ROXY Exceed User Manual 211 0010 Edition 4 2020...

Страница 2: ...man word and device and Whatman word only are trademarks of Whatman international Ltd SOLVENT IFD and AQUEOUS IFD are trademarks of Arbor Technologies Inc Clarity DataApex are trademarks of DataApex L...

Страница 3: ...ements for electrical equipment for measurement control and laboratory use part 2 010 Particular requirements for laboratory equipment for the heating of materials EN 61326 1 2013 Electrical equipment...

Страница 4: ...hutting down the system 37 ROXY Exceed control 39 Introduction 39 Overview of ROXY Exceed screens 40 Parameters 45 Dialogue Elite 50 Chromeleon CDS 52 Operation modes Parameters 53 Three or two electr...

Страница 5: ...CHAPTER 1 Table of contents 5 Digital I O connector 103 Chassis grounding stud 110 Troubleshooting 113 Instrument errors 113 Dummy cell test 115 Potentiostat accessories 121 Index 124...

Страница 6: ...6 211_0010 ROXY Exceed user manual rev 04...

Страница 7: ...ss of life or damage or destruction of parts or all of the equipment Do not proceed beyond a warning sign until the indicated conditions are fully under stood and met The caution sign denotes a hazard...

Страница 8: ...cturer for information concerning the decommissioning of equipment A device or system marked with CE fulfills the product specific requirements described in the European direc tives This is confirmed...

Страница 9: ...sive fluids and flammable liquids The instrumentation should only be oper ated by users with the following expertise Completed degree as chemical laboratory technician or comparable vocational trainin...

Страница 10: ...ed on the left site The symbol on the product indicates that the product must not be disposed as unsorted municipality waste Collection recycling information Please ship the instrument back to the man...

Страница 11: ...se of the system for any other purpose will cause unsafe sit uations System Operation To assure optimal performance keep of the potentiostat we recommend that the instrument is checked regularly and m...

Страница 12: ...on Manufacturer will not accept any liability for damage direct or indirect caused by connecting this instrument to devices and with cables which do not meet relevant safety standards Place the potent...

Страница 13: ...andling toxic or biologically infectious samples to pre vent bio hazards or hazards while working with the ROXY Exceed If ap plicable the instrument must be decontaminated before decommis sioning or s...

Страница 14: ...14 211_0010 ROXY Exceed user manual rev 04...

Страница 15: ...The ROXY Potentiostat is based on state of the art electronics with a large voltage range of 4 9 V and a push button electrode regeneration program Operational parameters and external equipment can be...

Страница 16: ...ument description ROXY Exceed Front side Description Description 1 Instrument housing 7 and value keys 2 LC tubing inlet outlet 8 Cursor keys 3 Instrument door panel 9 Door handle for opening door 4 4...

Страница 17: ...r panel 7 USB connector USB B 2 Type label pn sn etc 8 Fuse power rating 3 Digital I O connector 25 pins sub D fem 9 Mains switch inlet 4 Analog data 9 pins sub D fem 10 Grounding stud 5 Valve connect...

Страница 18: ...4 Door sensor 11 Mounting hole for column clamp M3 5 Mounting plate for cells columns 12 Fuse compartment 6 Column clamp 13 Door panel rear 7 Flow cell clamp for SenCell 14 Type label Note the shown...

Страница 19: ...cessful onsite installation of the instrument please arrange the following requirements at your location in advance Personal Computer In case the instrument is used via remote control by PC software D...

Страница 20: ...table for the following categories Installation category II Pollution degree 2 equipment class I Table I Environmental specifications Parameter Requirement Operating temperature 10 35 oC 50 104oF Maxi...

Страница 21: ...the following dimensions 44 D x 22 W x 43 H cm 17 3 D x 8 7 W x 16 9 H Take into account that additional space is necessary on all sides to prevent obstruction of ventilation holes and allow sufficie...

Страница 22: ...PS The mains supply must include a correctly installed protective earth conductor 3 The Roxy potentiostat is equipped with an universal AC DC switched mode power adapter rated for 100 240 V AC and 50...

Страница 23: ...by connecting this instrument to devices and with cables which do not meet relevant safety standards Chemicals Mobile phase and flush storage solutions must be clean as it is in direct contact with th...

Страница 24: ...t are included Prior to shipment your potentiostat has been thor oughly inspected and tested to meet the highest possible demands The results of all tests are included See check list below for referen...

Страница 25: ...hocks Do not place it near a source of heat or in direct sun light as this may influence the heating capabilities of the instrument Make sure the potentiostat is placed in such a way that the mains po...

Страница 26: ...nd protective earth The system must be connected to a suitable mains power supply with a correctly installed protective earth conductor Never use the system without a properly connected protective ear...

Страница 27: ...taskbar and open the menu Network Internet settings Alterna tive open Windows start menu open Setting menu and open Net work Internet menu 2 Open the menu Change adapter settings on the right panel of...

Страница 28: ...in your PC and click on properties to open the Network card setting 4 Open the menu Internet Protocol Version 4 TCP IPv4 menu double click 5 Configure the network IP address and subnet mask as depicte...

Страница 29: ...ed on the photograph 9 Switch on the ROXY Exceed Set the potentiostat temperature to 35 C if an Operational Qualification OQ will be executed or set it to the tempera ture at which your ROXY applicati...

Страница 30: ...his is by no means a replacement of the installa tion documentation available for the software packages Please refer to the software documentation for details Ensure you have Administrator access righ...

Страница 31: ...of all relevant fluidic connections are described to be able to use the ROXY Exceed to perform REDOX re actions When working with mobile phase solutions take the following pre cautions Use proper eye...

Страница 32: ...plete set of dedicated tubing assemblies LC connection kits tailor made for the application and syringe pump except the ROXY HDX system Flow cells Consult your EC flow cell manual for installation det...

Страница 33: ...ly partly or not at all filled with mobile phase containing electrolyte e g ammonium formate formic acid 3 the outside of the flow cell is wet particularly the part between the auxiliary and working e...

Страница 34: ...king conditions will never be obtained if the cell is switched ON with only water or another non conducting mobile phase Also be sure that no air bubbles are trapped in the electrochemical cell 2 Set...

Страница 35: ...to be Executed Periodic check of the oven temperature The operator should check verify on a daily basis if the actual oven tem perature is in accordance with the set temperature of the ROXY Exceed Fl...

Страница 36: ...y dust on the protective screens that cover the fans in the oven compartment Replacement of fuses Replace blown fuses with fuses of proper type and rating as stipulated on the rear panel and specified...

Страница 37: ...0 Acetonitrile water Take out the column mount the corresponding end caps and store the column in an appropriate place Flush and store the system with 50 water acetonitrile or methanol Switch the inje...

Страница 38: ...38 211_0010 ROXY Exceed user manual rev 04...

Страница 39: ...screen s of appearance The nature of an item can be 1 Control parameters with a cursor box can be attained via cursor buttons and changed by the value button 2 Status without a cursor box a parameter...

Страница 40: ...40 211_0010 ROXY Exceed user manual rev 04 Overview of ROXY Exceed screens DC mode...

Страница 41: ...Chapter 4 ROXY Exceed control 41 Pulse mode...

Страница 42: ...42 211_0010 ROXY Exceed user manual rev 04 SCAN mode...

Страница 43: ...Chapter 4 ROXY Exceed control 43 CONFIG menu...

Страница 44: ...44 211_0010 ROXY Exceed user manual rev 04 DIAG menu...

Страница 45: ...version S CELL ON OFF dc stat pulse stat scan setup scan stat Toggles between cell ON and OFF Confirmation is required Switch cell on off Switching on resets the clock to 0 00 Pulse mode pulsation occ...

Страница 46: ...n C Ec run dc only scan stat dur ing scanning Reflects the set cell potential Dis plays the actual cell potential in the scan mode S Filt DC mode dc setup dc stat Filter settings RAW 100 Hz Off 10 Hz...

Страница 47: ...the injector with this function button F S KEYB test Enters KEYB screen for key board test Press 2x F1 to leave F MARK dc stat pulse stat Triggers a marker signal on out put F MaxComp dc setup pulse s...

Страница 48: ...prog pulse setup1 pulse stat scan setup scan stat Range setting varying from 10 pA to 200 A full scale in 1 2 and 5 steps In the pulse and scan mode 10 nA to 200 A full scale can be used C S scan set...

Страница 49: ...p pulse setup1 Controls the temperature of the oven Range off 15 60 C se lectable in 1 C steps The oven is stable from 7 C above ambient C ts pulse setup2 Controls the duration of the sam pling time i...

Страница 50: ...delivery of sample solution Fig 7 ROXY Exceed potentiostat window in Dialogue Elite DC mode On the potentiostat tab the main measurement conditions can be set con trolled measurement mode potential s...

Страница 51: ...alogue cannot be considered as fully featured chromatography software package The free demo version of this program has already all functionality implemented functionality is unlocked by a license don...

Страница 52: ...lines Running a Time table enables time based automated parametric control of the Exceed potentiostat This is particularly useful when during a run parameters such as the cell potential settings have...

Страница 53: ...mpensates for polarization effects at the electrodes At the WE which is kept at virtual ground the electrochemical reaction takes place i e electrons are transferred at the WE This results in an elect...

Страница 54: ...the WE without AUX the working potential would be very well defined However the potential of a REF is only well defined if the current drawn is extremely low pico amperes resulting in a very limited d...

Страница 55: ...al from the I E converter before AD conversion is available via the Analog data output connector This output can be selected in the CONFIG menu by setting the parameter Output I E Dual flow cell contr...

Страница 56: ...an be a ReactorCell or PrepCell The LC channel can consist of a single syringe pump for delivery of target compound or a complete U HPLC setup with injector and column Parallel mode detection In paral...

Страница 57: ...a ble to use PC control from the Clarity Chromatography software or Dia logue Exceed software when working with 2 flow cells Fig 15 ROXY Exceed main menu top with active cell indicator in top right co...

Страница 58: ...p 100 mA 1 250 mA 2 5 A 25 A 50 mA 250 mA 2 A 25 A 20 mA 250 mA 1 A 25 A 10 mA 25 mA 500 nA 25 A 5 mA 25 mA 200 nA 25 A 2 mA 25 mA 100 nA 250 nA 1 mA 2 5 mA 50 nA 250 nA 500 A 2 5 mA 20 nA 250 nA 200...

Страница 59: ...A 25 mA 2 A 25 A 1 mA 2 5 mA 1 A 25 A 500 A 2 5 mA 500 nA 25 A 200 A 2 5 mA 200 nA 25 A For caption 1 and 2 see explanation below Table II When using Dialogue Elite software to control and operate the...

Страница 60: ...rent signal High frequency noise is efficiently re moved with ADF and will result in a less noisy current signal Fig 18 Signal to noise ratio is improved using a filter A vs B DC mode In the tables be...

Страница 61: ...RAW at 10 Hz Pulse mode In the pulse mode the working electrode is dynamically and continuously regenerated by a series of potential steps in a cyclic manner Data is pro cessed differently and the dat...

Страница 62: ...a sensitive range even if the background cell current is high For example with a background current of 20 nA one can still do measure ments in the 1 nA range because the maximum compensation for that...

Страница 63: ...0 With the compensation ON the full measurement range of 5 nA is available for the measurement peak 2 In case an Autozero Offset or a change of range is initiated on an instable or changing current si...

Страница 64: ...mode In Direct Current DC mode a static potential is constantly applied to the EC flow cell to establish an electrochemical oxidation or reduction reaction of a target compound In DC mode the resulti...

Страница 65: ...of conversion efficiency of the electrochemical reaction Pulse mode Besides the DC mode the ROXY Exceed can also be operated in Pulse mode The pulse mode is quite different from the DC mode Instead of...

Страница 66: ...on metal electrodes the activation energy barrier for the reaction is lowered allowing oxidation reduction at much lower po tential Due to the fact that the reactant remains at the WE surface or a met...

Страница 67: ...e current is measured is applied at the end of E1 Pulse mode 2 In the ROXY Exceed an extended pulse mode pulse mode 2 is available when operating the instrument via a PC using Dialogue Elite or Chro m...

Страница 68: ...ew pulse mode 2 with freely programmable t E table In red the sampling of data for acquisition Scan mode See next chapter describing the optimization of the working potential In Pulse mode 2 the ADF f...

Страница 69: ...l target compounds and reaction products should be sufficiently separated under the applied LC conditions A scanning voltammogram is obtained in the so called scan mode of the ROXY Potentiostat in the...

Страница 70: ...cal current that is am plified by the controller The mechanism of the REDOX reactions is the same for the ROXY appli cations The potential is the reactions driving force but the mass spec trometry MS...

Страница 71: ...tio is obtained Additionally the hydrodynamic voltammogram can be used to optimize po tential when ROXY EC LC system is used The drug compound xenobiotic is oxidized in the electrochemical cell to the...

Страница 72: ...etry potential waveform The current is plotted against the working potential to give a voltammo gram I E curve An example is shown in Fig 29 A difference with a hy drodynamic is that in scanning volta...

Страница 73: ...tagnant double layer exists where molecular transport takes place by diffusion only Therefore the current at and beyond this potential is called the diffusion limited current Fig 29 Scanning voltammet...

Страница 74: ...ted at every point during the analysis The optimal potential can be estimated from EIC plots With help of the Fig 29 where EICs are presented it is easy to estimate the potential range in which the de...

Страница 75: ...est difference in peak height In the example of Fig 32 the selectivity for compound X is improved consid erably by decreasing the potential to E2 or E1 Obviously if compound Y is the compound of inter...

Страница 76: ...tial at higher pH When the working potential is high E2 and the signal is diffusion limited an increase in pH will result only in a small increase of the peak height When the working potential is lowe...

Страница 77: ...nd current is read from the display of the potentiostat I cell and the noise is measured 3 The run is started by injecting the compound When at the high working potential no signal is obtained it may...

Страница 78: ...sen Fig 35 Programming the scan mode in the SCAN SETUP screen With the Dialogue Elite control software a scanning voltammogram can be programmed under the Potentiostat tab in the main window Fig 36 Pr...

Страница 79: ...2 until the predefined number of scans programmed are completed Note that under Dialogue Elite control also a stand by potential E standby can be programmed This is the potential at which the cell be...

Страница 80: ...In the figure below a scan ning voltammetry set up is shown Fig 38 ROXY Exceed scanning voltammetry set up with a syringe pump The Antec dual syringe infusion pumps pn 188 0035 36 and 37 which can be...

Страница 81: ...syringe pump for direct infusion of analyte in the flow cell Prepare a solution of the pure compound dissolved in preferably the HPLC buffer with a concentration in the range of 10 100 M Set the lower...

Страница 82: ...b A typical flow rate to start with is 10 L min Optimize the flow rate if required during the scan experiments Start the syringe pump and before scanning assure that the flow cell is sufficiently prim...

Страница 83: ...voltammogram visualizes the ion abundance versus m z as a function of applied potential to the electrochemical cell With a mass voltammogram the optimal potential can be determined for electrochemica...

Страница 84: ...of MS software Both 3 D and 2 D MS Voltammograms were acquired in the DC mode The Dialogue controls the syringe pump the potentiostat and triggers the acquisition of mass spectra at the designated ce...

Страница 85: ...on flat smooth surface keep space under the potentiostat free Power requirements 100 240 VAC 50 60 Hz 260 VA auto sens ing Mains fuse 2 5 AT 250V 5x20 mm IEC 60127 2 For safety reasons any other inte...

Страница 86: ...Female Analog output 1x 25 pins sub D Female Digital I O Analog output DAC 1 to 1 V full scale via 16 bit D A converter Analog output I E 2 5 to 2 5 V full scale unprocessed I E con verter signal Dig...

Страница 87: ...ion Hz Waveform Free programmable multi step waveform with up to 30 time potential t E coordinates and max pulse duration of 4 s Time points in 10 ms increments Sampling time Sampling interval is free...

Страница 88: ...Cell volume Approximately 0 75 l with 50 m spacer WE electrodes Glassy carbon GC Boron Doped Diamond BDD gold Au platinum Pt Optional silver Ag and copper Cu Reference electrode HyREF Pd H2 Auxiliary...

Страница 89: ...DD Platinum Pt and Gold Au Reference electrode HyREF Pd H2 electrode Auxiliary electrode Conductive PEEK PEEK 30 carbon fiber rein forced Wetted materials PEEK Carbon Methyl vinyl silicone rubber Sili...

Страница 90: ...volume 10 l effective spacer thickness 50 m Counter electrode Platinum Pt Inlet block WE Titanium Ti Wetted materials Titanium Platinum Methyl vinyl silicone rubber Silicone VMQ 70 or PTFE PEEK Fluidi...

Страница 91: ...RGC Optional Flat Smooth Boron Doped Diamond BDD and Tubular Mesh Platinum PT Reference electrode HyREF Pd H2 electrode Optional Ag AgCl reference electrode Auxiliary electrode Coiled platinum wire in...

Страница 92: ...92 211_0010 ROXY Exceed user manual rev 04...

Страница 93: ...hapter all rear panel functionality is described The ROXY Exceed has besides the mains inlet in total 5 connectors on the rear panel for com munication data output and I O A photo of the rear panel co...

Страница 94: ...e installer software utility Fixed communication baud rate 921600 bps Communication over LAN is used for parametric instrument control and data acquisition Please consult the installation section for...

Страница 95: ...out is established by con necting the LOAD INJ sensor wires leads of a manual valve to pin 5 and 6 contact closure Inject marker A connected valve enables the inject marker pin 9 The contact is high...

Страница 96: ...e device set tings window EC device and valve control buttons will appear in the po tentiostat window Fig 45 Dialogue Elite device settings window Fig 46 ROXY Exceed potentiostat window with Valve con...

Страница 97: ...k box Fig 47 Dialogue Elite device settings manual valve check box Valve status control In stand alone mode Exceed only the valve status for both an electrically actuated valve and manual valve is dis...

Страница 98: ...alve control is possible with this type of valve Fig 48 Example of the valve flow path of a 6 port valve In Dialogue Elite the valve status position is shown under the monitor tab To make it visible i...

Страница 99: ...47 Note that the valve will switch immediately after a change from Load to Inject checkboxes or vice versa no Send to device action is required An electrically actuated VICI valve can also be control...

Страница 100: ...the instrument The ANALOG DATA con nector D9 female can either be connected to an X Y recorder or A D con verter The ANALOG DATA output can supply either a non manipulated signal directly from the I...

Страница 101: ...100 and 10 in the I E converter circuit The output parameter Vout source can also be selected set using Dialogue Exceed Go to the device settings menu and Acquisition tab and set the analogue output t...

Страница 102: ...put of 250 mV in the 200 nA range cor responds with an actual cell current of 250 1000 200 nA 50 nA I E output The I E output is the unprocessed analog signal from the I E converter cir cuit This sign...

Страница 103: ...is shown in the table below Table VII Analog data output connector lay out Pin Layout 1 Vout 1 2 Vout 2 3 Vout 3 4 Vout 4 5 Vout 5 6 9 GND To measure for example the analog signal of cell 1 with an ex...

Страница 104: ...3 common Relay2 pin 4 normally closed pin 5 normally open pin 6 common The maximum rating for these contact closure outputs are 24 VDC switch ing voltage and 0 25 A The relays can be controlled in the...

Страница 105: ...o a value within the measure ment range again The overload output pin 11 is one of the configurable I O s The configurable I O s can be programmed in the IO menu which is a sub menu of the CONFIG menu...

Страница 106: ...inputs are 1 2 and all In case all is selected all cells present in the ROXY Ex ceed will be switched on or off when the corresponding input is triggered Autozero The ROXY Exceed has 2 TTL inputs pin...

Страница 107: ...uts checkbox under the controls section Fig 54 Dialogue Exceed Potentiostat tab with I O status and control but tons check boxes The status of the Relays and TTL inputs can be set to active or inac ti...

Страница 108: ...sure to pro gram a second step to inactivate the Output again and put it back in its ini tial inactive state again Fig 55 Dialogue Exceed Event Editor window Programming of output A Fig 56 Dialogue Ex...

Страница 109: ...2 Active in case of signal over load OUT OF RANGE PAD OVLD 12 TTL IN Cell on 1 A 1 2 Trigger to switch the cell on 13 TTL IN Cell on 2 Trigger to switch the cell on 15 TTL IN Cell off 1 A 1 2 Trigger...

Страница 110: ...ostat rear panel subsequently connect the I O connector board to the end of the I O cable Fig 57 Left ROXY Exceed rear panel with I O screw terminal board in stalled On the rear side of the I O conne...

Страница 111: ...f the in strument can be used for shielding purposes For example to shield the flow cell from other equipment which might be coupled in series with the electrochemical potentiostat such an MS Fig 58 L...

Страница 112: ...112 211_0010 ROXY Exceed user manual rev 04...

Страница 113: ...or several hardware fault conditions which will be shown in the instruments LCD display Table IX Error messages Error Message 11 Checksum error 12 Temperature sensor 1 error 13 Disconnect flow cell x...

Страница 114: ...Charging current in pulse mode out of range Pressing AZERO may give an adequate read out again If not it is advisable to change the pulse settings increase t1 or use a less sensitive range Make sure...

Страница 115: ...al behavior With high substrate concentrations it can be normal behavior Check with solvent without substrate if current is at expected value and in scale Increase range if possible Erratic cell cell...

Страница 116: ...and maintenance checks The dummy cell test can be performed standalone via the LCD display in combination with an A D converter ROXY Exceed only or via the Dia logue Exceed DataApex Clarity software A...

Страница 117: ...could be wrong with the potentiostat hardware Please consult your local representative Internal dummy cell The ROXY Exceed also has the option to run a so called internal dummy cell test This exclusi...

Страница 118: ...all the parameters to the values listed in Table XI and set the cell to OFF Subsequently click the Send to device button Evaluate the cell current in the monitor window The cell current shown in the...

Страница 119: ...um current which can be compensated in these ranges is 25 A See table II and III in Chapter 3 for an overview of the maximum compensation for all selectable ranges in the DC and pulse mode 3 SCC DCC I...

Страница 120: ...120 211_0010 ROXY Exceed user manual rev 04...

Страница 121: ...12 mm 250 0113 Fuse 2 5 AT 250 V 250 0170 LAN UTP cable crossed 3 meter 250 0175 USB cable A B 3 meter 250 0131B I O conn Board 250 0131C I O cable 25M 25M 1 8m 250 0032X ROXY Exceed trigger cable 250...

Страница 122: ...at high voltages of typically 3 5 kV In cases where the inlet of the ESI MS is not grounded the grounding kit pn 250 0035 must be used If not used it may lead to damage of the ROXY Exceed potentiosta...

Страница 123: ...an MS Check the technical documentation of your specific MS for details how to make the connections on the MS The black wire on the cable should be connected to ground The input lead with screw termi...

Страница 124: ...ummy cell external 108 internal 109 E1 control 44 E2 control 44 Electrical safety 10 electrochemical reaction 66 Elite Dialogue software 28 EN 55011 group 1 class A ISM equipment 24 Environmental spec...

Страница 125: ...lectrode 51 ROHS 9 RS232C 113 S N ratio 73 Safety instructions 10 scan mode example 74 scanning voltammogram 68 Serial mode detection 54 Solvents 11 specifications DECADE Elite 81 87 Symbols 7 System...

Страница 126: ...126 211_0010 ROXY Exceed user manual rev 04 Working environment safety 10...

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