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Antec Scientific ROXY 210 User Manual

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Antec Scientific
Industrieweg 12
2382 NV Zoeterwoude
The Netherlands
ROXY Potentiostat
User manual
210.7010, Edition 09, 2018
T +31 71 5813333 | info@AntecScientific.com | www.AntecScientific.com

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  • Page 1 Antec Scientific Industrieweg 12 2382 NV Zoeterwoude The Netherlands ROXY Potentiostat User manual 210.7010, Edition 09, 2018 T +31 71 5813333 | info@AntecScientific.com | www.AntecScientific.com...
  • Page 2 Copyright ©2016, Antec Scientific, The Netherlands. Contents of this publication may not be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from the copyright of the owner. The information contained in this document is subject to change without notice.
  • Page 3 Chapter 1 Table of contents Declaration of conformity We Antec Leyden B.V., Zoeterwoude, The Netherlands, declare that the product: ROXY Potentiostat type 210 to which this declaration relates, is in conformity with the following CE directives: Low Voltage Directive (2014/35/EU) Safety requirements for electrical equipment for measurement, control, and laboratory use: - Part 1: General Requirements IEC61010-1 2...

  • Page 4: Warning Symbols

    ROXY Potentiostat user manual ed. 8 Warning Symbols The following symbols are used in this guide: This sign warns about the risk of electric shock. It calls attention to a procedure or practice which, if not adhered to, could result in loss of life by electrocution. Do not proceed beyond a danger sign until the indicated conditions are fully understood and met.

  • Page 5: Chapter 1 Table Of Contents

    Chapter 1 Table of contents The attention sign signals relevant information. Read this information. The note sign signals additional information. It provides advice or a suggestion that may support you in using the equipment. Intended use The ROXY potentiostat in combination with flow-through reactor (µ-PrepCell or ReactorCell) is used for controlled REDOX reactions up-front Mass Spectrometric detection.

  • Page 6: Weee Directive

    ROXY Potentiostat user manual ed. 8 Information on safety practices is provided with your equipment operation manuals. Before using your equipment or accessories, you must thoroughly read these safety practices. This manual is written for laboratory technicians skilled in the art. Unskilled, improper, or careless use of this equipment can create fire hazards, or other hazards which can cause death, serious injury to personnel, or severe damage to equipment and property.

  • Page 7: Chapter 1 Table Of Contents

    Chapter 1 Table of contents The ROXY potentiostat is ROHS compliant and in conformity with Directive 2011/65/EU Restricted use of Hazardous Substances in electrical and electronic Equipment (ROHS). Antec Leyden B.V. is an ISO 9001 certified company. Warranty, spare parts and service The warranty period of this instrument is 1 year on workmanship, wear and tear parts are excluded.

  • Page 8: Electrical Safety

    ROXY Potentiostat user manual ed. 8 Operation To assure optimal performance keep of the instrument we recommend that the flow cell is checked regularly and maintenance procedures are carried out. Preventive maintenance contracts are available for that Purpose. Please contact your local dealer or the nearest sales office for more information. Electrical safety The removal of protective panels on the instrument can result in exposure to potentially dangerous voltages.

  • Page 9: Chapter 1 Table Of Contents

    Chapter 1 Table of contents fuse holder is integrated in the mains connector. Ensure that the instrument is never put in operation with fuses of a different type. This could cause fire. Only use manufacturer-supplied I/O cable(s) to connect with other devices. Thoroughly connect shielding to common.
  • Page 10 ROXY Potentiostat user manual ed. 8 Waste disposal Perform periodic leak checks on LC tubing and connections. Do not close or block the drain in the oven compartment. Do not allow flammable and/or toxic solvents to accumulate. Follow a regulated, approved waste disposal program. Never dispose of flammable and/ toxic solvents through the municipal sewage system.

  • Page 11: Table Of Contents

    Chapter 1 Table of contents Table of contents Warning Symbols 4 Intended use 5 WEEE directive 6 Electrical safety 8 Table of contents 11 ROXY Potentiostat 13 Installation guide 15 Storage requirements 15 Site Preparation Requirements 15 Personal Computer 15 Environmental requirements 16 Size Requirements 17 Electrical and power requirements 18...
  • Page 12 ROXY Potentiostat user manual ed. 8 Overload 46 Auto zero 46 To pos I, L 46 Cell on, off 46 Optimization of working potential 49 Introduction 49 Electrochemical reactions 49 Hydrodynamic and scanning voltammogram 50 Optimisation using a voltammogram 54 Electrochemical detection 54 On-line electrochemistry mass spectrometry 56 Construction of a hydrodynamic voltammogram 58...

  • Page 13: Roxy Potentiostat

    Chapter 1 ROXY Potentiostat C H A P T E R ROXY Potentiostat Congratulations on your purchase of the ROXY Potentiostat. With more than 20 years of experience in Electrochemistry (EC), Antec introduces a new, dedicated Potentiostat for on-line EC/MS and EC/LC/MS. The ROXY Potentiostat generates metabolites of drugs or xenobiotics, similar to those generated during in vivo metabolic processes, in a significantly shorter time span (seconds vs.
  • Page 14 ROXY Potentiostat user manual ed. 8...

  • Page 15: Installation Guide

    CHAPTER 2 Installation guide C H A P T E R Installation guide It is evident that (for as far it is not specified in this document) the installation site must comply with all applicable local laws and regulations with regard to electrical and mechanical installations, building safety, and use of potentially hazardous materials/chemical and disposal thereof, etc.

  • Page 16: Environmental Requirements

    ROXY Potentiostat user manual ed. 8 Computer requirements can be downloaded from website (www.antecscientific.com) Installing software requires a computer with administrator access. Make sure that the PC and its USB ports is authorized/able to install third-party software. Inform your IT department well in advance to arrange authorization to avoid unnecessary delays during the installation.

  • Page 17: Size Requirements

    CHAPTER 2 Installation guide For optimum performance it is recommended that the ambient temperature of the laboratory be between 18-25 °C and be held constant to within ± 2 °C throughout the entire working day. Note: that for optimal performance of the oven the oven temperature should be set at least 7 degrees higher as ambient temperature.

  • Page 18: Electrical And Power Requirements

    ROXY Potentiostat user manual ed. 8 Tip: Installation of the ROXY potentiostat + PC on a suitable movable laboratory cart/table has multiple advantages: - Easy access to all sides of the instrumentation - System can be easily manoeuvred next to the (ESI inlet) MS - Flexibility with respect to use of both ROXY potentiostat and MS.

  • Page 19: Chemicals

    CHAPTER 2 Installation guide For regions with deviating mains plugs/sockets like (for example UK, Switzerland, Brazil etc.) make sure to have the appropriate power cords available on-site at the date of installation. Make sure these power cables are properly grounded and meet the relevant safety standards which apply in your country.

  • Page 20: Unpacking

    ROXY Potentiostat user manual ed. 8 Unpacking Inspect the transport box for possible damage as it arrives. Immediately inform the transport company in case of damage, otherwise she may not accept any responsibility. Keep the transport box as it is designed for optimum protection during transport and it may be needed again.

  • Page 21: Lc Connections

    CHAPTER 2 Installation guide Install the potentiostat in an area which meets the environmental conditions listed below, for further requirements read the : Table I. Environmental conditions Parameter Requirement 10 – 35 C (50 – 95 °F) Operating temperature Maximum Altitude 2000 meter (7500 ft) 20 –...
  • Page 22 ROXY Potentiostat user manual ed. 8 connectors are marked with a label for identification. The cell connector inside the oven compartment is ESD sensitive. Make sure that the electrochemical cell is OFF when removing or connecting the cell cable. Never switch ON the electrochemical cell when: - the cell cable is not correctly connected - the cell is only partly (or not at all) filled with mobile phase containing the supporting electrolyte (e.g., ammonium formate, formic acid)

  • Page 23: Maintenance & Shutdown

    CHAPTER 3 Maintenance & Shutdown C H A P T E R Maintenance & Shutdown Maintenance In this paragraph all maintenance is described which can be performed by the end-user, all other maintenance & service procedures may only be performed by authorized service engineers only.

  • Page 24: Replacement Of Fuses

    ROXY Potentiostat user manual ed. 8 crusts (in case of buffered mobile phases), which could block the drain in the bottom of the cell cabinet. Remove any 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 in the installation section of this manual.

  • Page 25: Shutting Down The System

    CHAPTER 3 Maintenance & Shutdown Shutting down the system There are a couple of steps to take to switch off an system with potentiostat for a longer period of time. Shutting down is not different from most other HPLC systems. Perform the following procedure: •...
  • Page 26 ROXY Potentiostat user manual ed. 8...

  • Page 27: Roxy Potentiostat

    CHAPTER 4 ROXY Potentiostat C H A P T E R ROXY Potentiostat Introduction The ROXY Potentiostat has been designed for maximum functionality and ease of use. The control of EC parameters is such that without reading this chapter, it should be possible to operate the potentiostat.

  • Page 28: Overview Of Roxy Potentiostat Screens

    ROXY Potentiostat user manual ed. 8 Overview of ROXY Potentiostat screens V o u t = + 0 . 0 5 7 V = + 2 3 . 4 5 n A R a n g e = 5 0 n A = + 0 .
  • Page 29 CHAPTER 4 ROXY Potentiostat V o u t = + 0 . 0 5 7 V = + 2 3 . 4 5 n A P U L S E R a n g e = 5 0 n A = + 0 .
  • Page 30 ROXY Potentiostat user manual ed. 8 V o u t = + 0 . 0 5 7 V = + 2 3 . 4 5 n A S C A N R a n g e = 5 0 n A = + 1 2 0 1 m V R E M O T E C o m p = o f f...
  • Page 31 CHAPTER 4 ROXY Potentiostat A N T E C M A I N R O X Y P o t e n t i o s t a t 5 . 0 2 C O N F I G > D C >...

  • Page 32: Parameters

    ROXY Potentiostat user manual ed. 8 Parameters Explanation: Type S is status, F is function and C is control.
  • Page 33 CHAPTER 4 ROXY Potentiostat Parameter screen Description Type 28 > 30˚C dc stat Displays the actual (left value) and the pulse stat pre-set oven temperature (right value). scan stat prog Adds the active data line to the time file . Confirmation is asked for if an existing time is overwritten.
  • Page 34 ROXY Potentiostat user manual ed. 8 Parameter screen Description Type Displays the cycle counter. If a time file has to be executed more than once (‘Cycles’>1), this is the number of times a time file has been started (see page 43). RESET (external) or QUIT sets Cy to 1 and returns to EVENTS SETUP screen.
  • Page 35 CHAPTER 4 ROXY Potentiostat Parameter screen Description Type EndCycle prog Enters a screen to set EndCycleTime. Controls duration of a time file (max. 999.99 min). When this time is reached the execution of the time file stops. If programmed, the next run is started. Cannot be smaller than smallest time in time file +0.01 min.
  • Page 36 ROXY Potentiostat user manual ed. 8 Parameter screen Description Type Enters ‘KEYB’ screen, for keyboard KEYB test test. Press 2x F1 to leave. MARK dc stat, Triggers a marker signal on output. pulse stat MaxComp dc setup, Maximum cell current that can be pulse setup1 compensated for using auto zero.
  • Page 37 CHAPTER 4 ROXY Potentiostat Parameter screen Description Type START run, scan In DC and pulse mode: toggle between stat STOP and START execution of a time file . Starts a scan in scan mode. STOP run, scan Scan mode: STOP aborts scan and stat resets cell potential to E1.
  • Page 38 ROXY Potentiostat user manual ed. 8 Parameter screen Description Type pulse setup2 Controls the duration of the sampling time in the pulse mode. The time can be set between 20 and 100 ms in 20 ms increments. Tsensor system Displays active temperature sensor Valve prog Controls the electrically actuated...

  • Page 39: Roxy Potentiostat Data Systems

    CHAPTER 4 ROXY Potentiostat ROXY Potentiostat data systems The ROXY Potentiostat in the ROXY EC system can be fully controlled by Dialogue Elite™ software (Fig. 9). Additionally, Dialogue Elite can control syringe pump, which is delivering sample solution. The software package contains a set of event table files (*.evt) for the automated recording of mass voltammograms and sample oxidation or reduction.
  • Page 40 ROXY Potentiostat user manual ed. 8 Fig. 10. Dialogue for ROXY. Events programming window. The ROXY Potentiostat (delivered before 2013, with FW5.11) in ROXY EC/LC system is controlled by Clarity software (Fig.11). Programming of all functions of the potentiostat is performed in the Clarity: Main, Output and Time Table tabs of the Potentiostat control window.
  • Page 41 CHAPTER 4 ROXY Potentiostat Fig. 11. Clarity software. The potentiostat control window. ROXY potentiostats delivered after 2013 with updated electronics (which can be recognized by its FW version: FW 5.2x or higher) cannot be controlled in Clarity. For this instrument Dialogue Elite should be used for remote control.
  • Page 42 ROXY Potentiostat user manual ed. 8...

  • Page 43: Events And Time Files

    CHAPTER 5 Events and time files C H A P T E R Events and time files Introduction Running an Events table (time file) enables a time-based, automated and full parametric control of the analysis. This is particularly useful when during a run or between runs settings have to be changed such as the sensitivity, auto zero or control of external equipment (i.e.
  • Page 44 ROXY Potentiostat user manual ed. 8 potentiostat. For some reason, a user wants to give an –30% offset after t=5.00 min. Go from MAIN, DC SETUP to DC STAT screen to see if the cell is ON or not. Set the cell to the desired status and return to DC SETUP. From the DC SETUP screen select 'EVENTS'.

  • Page 45: Output Events

    CHAPTER 5 Events and time files 00% to prepare for the next run. An auto zero event is programmed 0.02 min later at Time = 14.98 min. After entering all events, press PREV (or ENDCYCLE) to enter the EndCycle screen. Program the EndCycleTime. This time is always 0.01 min higher than the last programmed events.

  • Page 46: Overload

    ROXY Potentiostat user manual ed. 8 contact is high when the valve is in ‘load’ position, and low in the ‘inject’ position. It can be used to start the integration software when injection is done. Overload Activated when a overload occurs, see also page 63 for details. Auto zero Enables external activation of the auto zero command.
  • Page 47 CHAPTER 5 Events and time files Table IV. I/O contacts connector B. Name Function 1 - 3 Common Ground Free TTL input Mark Baseline spike of 10% FS, duration: 0.1 s Status I Status read of electric valve, pos B (inject) Status L Status read of electric valve, pos A (load) 8 - 11 Common...
  • Page 48 ROXY Potentiostat user manual ed. 8...

  • Page 49: Optimization Of Working Potential

    CHAPTER 6 Optimization of working potential C H A P T E R Optimization of working potential Introduction A current - voltage (I/E) relationship (Electrochemical Detection), or voltammogram (ROXY applications), characterizes an analyte. It gives information on the optimum working potential, which can be used to improve detection sensitivity and selectivity or REDOX products formation.

  • Page 50: Hydrodynamic And Scanning Voltammogram

    ROXY Potentiostat user manual ed. 8 needed to initiate or enhance the electrochemical reaction. Different analytes may have different oxidation or reduction potentials. Fig. 13. Oxidation/reduction reaction of norepinephrine. The mechanism of the REDOX reactions is the same for the ROXY applications.
  • Page 51 CHAPTER 6 Optimization of working potential ion chromatogram (EIC) representing m/z ratios (mass to charge) of specific metabolites will be plotted and the optimal potential can be estimated. Fig. 14. Hydrodynamic voltammogram of norepinephrine (A) at a glassy carbon working electrode, and the current of the baseline (B). At E the electrochemical signal becomes diffusion limited (Example with ECD).
  • Page 52 ROXY Potentiostat user manual ed. 8 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. 15. Scanning voltammetry of 1.0 mol/l norepinephrine (A) at a glassy carbon working electrode, at a scan speed of 10 mV/s.
  • Page 53 CHAPTER 6 Optimization of working potential (1200 mV) should be applied. In figure 17 the different mass spectra represents the different conditions: no potential, 300 mV or 1200 mV, respectively. The mass spectra corresponds to the scanning voltammogram presented in the figure 17.

  • Page 54: Optimisation Using A Voltammogram

    ROXY Potentiostat user manual ed. 8 Optimisation using a voltammogram Electrochemical detection Sometimes, when interfering peaks appear in the chromatogram, it is possible to optimize the method with regard to selectivity. If the interfering compound has a higher oxidation potential, a working potential is chosen that gives the best selectivity, i.e.
  • Page 55 CHAPTER 6 Optimization of working potential and the signal is not diffusion limited, the signal will strongly increase at higher pH. In both cases the background current increases at a higher pH. Fig. 19. At a higher pH the I/E curve of norepinephrine is shifted to the left. Reaction kinetics predict that electrochemical detection is mass flow dependent.

  • Page 56: On-Line Electrochemistry Mass Spectrometry

    ROXY Potentiostat user manual ed. 8 background signal is sensitive towards fluctuations in the flow rate. Therefore, it is important to use a pulse-free solvent delivery system. Fig. 20. Construction of a hydrodynamic voltammogram for norepinephrine. Chromatograms are obtained at cell potentials ranging from 1.0 V (back) to 0.4 V (front), with 100 mV steps.
  • Page 57 CHAPTER 6 Optimization of working potential and in this case the potential should be ca. 1200mV. For each cell potential mass spectra are recorded and saved in separate data files. Fig. 21. 3-D MS Voltammogram of Amodiaquine. The plot is reconstructed from the separate mass spectra saved for each potential value.

  • Page 58: Construction Of A Hydrodynamic Voltammogram

    ROXY Potentiostat user manual ed. 8 Construction of a hydrodynamic voltammogram Before a hydrodynamic voltammogram can be obtained, the chromatographic conditions should be optimized. Then the following steps are taken: A solution of the analyte at a concentration between 1 - 100 mol/l, is prepared in mobile phase.
  • Page 59 CHAPTER 6 Optimization of working potential scan, i.e. from 0.2 V to 1.2 V and back to 0.2 V. In the continuous mode the voltage is swept up and down between both potentials. Fig. 24. A continuous scanning voltammogram in Dialogue Elite software. Example of multiple scans (‘continuous’) of Amodiaquine.
  • Page 60 ROXY Potentiostat user manual ed. 8 Fig. 25. Scan settings window (under detector tab) in Dialogue Elite software.

  • Page 61: Specifications Roxy Potentiostat

    CHAPTER 7 Specifications ROXY Potentiostat C H A P T E R Specifications ROXY Potentiostat General specifications *) Specifications marked with * are only valid for the ROXY potentiostat high current version. For the previous model the max current range is 200µA for all measurement modes. The noise specification of the previous model is <...

  • Page 62: Pulse Mode

    ROXY Potentiostat user manual ed. 8 PULSE mode 10 nA – 20 mA* in 1, 2, 5 steps Range 0.5 – 0.01 Hz in 1, 2, 5 steps Filter (cut off) Pulse times t1: 100 - 2000 ms; t2: 0 - 2000 ms; t3: 0 - 2000 ms in 10 ms steps Sample times 20 ms - (t1 - 60 ms), with 20 ms increments...
  • Page 63 CHAPTER 7 Specifications ROXY Potentiostat µ-PrepCell Type Thin-layer electrochemical cell (micro-preparative work) Spacers 50 or 100 µm, stainless steel, stackable (max. stack thickness 250 µm) WE dimensions 12 x 30 mm, thickness 1 mm WE area (wetted) 1.9 cm Cell volume 10 µl (effective spacer thickness 50 µm) Working electrode Glassy Carbon (GC), Boron-Doped Diamond (BDD),...
  • Page 64 ROXY Potentiostat user manual ed. 8...

  • Page 65: Error Messages

    CHAPTER 8 Error messages C H A P T E R Error messages Table V. Error messages. Error Message Incompatible boot version Control board error Sensor board x error (x = board number) Firmware program error Record error Incompatible FW version Incompatible FW Control board FW erase failed Sensor board x...
  • Page 66 ROXY Potentiostat user manual ed. 8...

  • Page 67: Rear Panel

    CHAPTER 9 Rear panel C H A P T E R Rear panel Connectors A, B and C For detailed information on the I/O contacts see page 46. Fig. 26. ROXY Potentiostat rear panel. RS232C The RS232 interface provides full parametric control from a PC. Programmable parameters comprise cell potential, range, auto zero, offset, filter, electrical injector and control of ROXY Potentiostat output contacts for control of external equipment.
  • Page 68 ROXY Potentiostat user manual ed. 8 locked. Keeping the PREV button (F1) pressed for 4 seconds disconnects from RS232 control and returns to MAIN. V o u t = + 0 . 0 5 7 V = + 2 3 . 4 5 n A R a n g e = 5 0 n A = + 0 .

  • Page 69: Troubleshooting Guide

    CHAPTER 10 Troubleshooting guide C H A P T E R Troubleshooting guide No response, no product in MS Possible cause Remedy No power Check line voltage setting, plug in power cord Power switch off Turn this switch ON (at the rear panel) Faulty fuse Replace fuse Cell disconnected, or...
  • Page 70 ROXY Potentiostat user manual ed. 8...

  • Page 71: Dummy Cell

    CHAPTER 11 Dummy cell C H A P T E R Dummy cell External dummy cell A successful dummy cell test confirms that the controller, including the cell cable, functions properly. If the result of the noise measurement with the dummy cell is within specs, the controller is excluded in a troubleshooting procedure.

  • Page 72: Internal Dummy Cell

    ROXY Potentiostat user manual ed. 8 Table VII. Dummy cell test settings. Parameter Setting Cell potential 800 mV Cell current 2.67± 0.05 nA (read-out) Oven 35 °C, stable Filter off (or as specified) Range 100 pA/V (or 1 nA/V) The results (cell current and noise) of the dummy cell test should be within the above mentioned test criteria.

  • Page 73: Potentiostat Accessories

    CHAPTER 12 Potentiostat accessories C H A P T E R Potentiostat accessories The electrochemical potentiostat is shipped together with a number of parts. The listing in Table below may not be complete, see check list of delivery for complete listing. Table VIII.
  • Page 74 ROXY Potentiostat user manual ed. 8 With a ROXY EC system (pn 210.0070) or ROXY EC/LC system (pn 210.0080C) this part is provided with the systems An ESI interface of an MS is usually operating at high voltages of typically 3 –...

  • Page 75: Triggering

    CHAPTER 12 Potentiostat accessories Trigger cable The ROXY potentiostat is delivered with 250.0032E ROXY potentiostat trigger cable. The trigger cable 15-pins d-sub connector marked ‘ROXY con A’ should be connected to connector A of sensor board 1 (the sensor board located above the control board) on the rear panel of the ROXY potentiostat.
  • Page 76 ROXY Potentiostat user manual ed. 8...
  • Page 77 CHAPTER 12 Potentiostat accessories...
  • Page 78 ROXY Potentiostat user manual ed. 8 Index...
  • Page 79 Auto zero, I/O contact, 46 AUX1, I/O contact, 46 AUX2, I/O contact, 46 Biological Hazard, 9 buttons ROXY keyboard, 27 Cell off, I/O contact, 46 Cell on (off), I/O contact, 46 cell on, I/O contact, 46 cleaning of detector, 24 Common, I/O contact, 46, 47 DC mode specifications, 61...
  • Page 80 ROXY Potentiostat user manual ed. 8 noise, 58, 61 Overload, I/O contact, 46 potential optimisation, 49 pulse mode specifications, 62 Relay 1, I/O contact, 46 Relay 2, I/O contact, 46 Reset, I/O contact, 46 RS232C, 67, 75 S/N ratio, 58 scan mode example, 58 scanning voltammogram, 51...

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