Dialogue for ROXY user guide, ed. 2
Contents
1. J ROXY Dialogue PT be eto File Edit Tools Options Data Ceni Cell2 1 Events ee Syringe pump settings LC 100 110 Settings G A Flow rate 10 000 uL min 2 ee Connect Volume 0 000 reset uL ml min mL hour Diameter 4 61 select mm Set Read Pump started Keybrd Direction Infused INF 664 05 uL Withdraw jan Start IT Auto connect at startup Stop 2173 2173 000186 4 Status default 32 cell present 1K ADC 8 Max 2 5 m DD Fig 3 Dialogue syringe pump settings window 8 Dialogue for ROXY user guide ed 2 Events The Events tab in Dialogue figure 4 offers the possibility to compose an event table for the execution of an automated sequence of parametric control events It is used for the automated recording of for instance a mass voltammogram with the ROXY EC system see next paragraph The event table consists of a series of data lines in which settings of the ROXY potentiostat or infusing pump can be changed with 0 01 min 0 6 s time resolution To start the execution of the command e Press Start in the Events tab If data acquisition is required e Check the box Start Stop with run e Goto pull down menu Options gt Start run data in excel file will be saved e Check the box Repeats to repeat the program if required type the number of repeats in the appropriate box The events can be opened and saved in File pull down menu The list of avai2. 2000 mV with 100 mV steps See Table 2 but the data will be saved in one MS file The sec ond program has the potential range up to 3000mV Mass spectrometry allows the sample identification determining the elemental composition structure elucidation and all ions having specific m z ratios are plotted in the mass spectrum Mass spectrometry data can be presented in form of mass chromatogram e g the extracted ion chromatogram EIC in which a specific metabolites oxidation products are monitored throughout the entire run and a particular analyte s mass to charge ratios are plotted at every point during the analysis The optimal potential can be estimated from EIC plots 16 Dialogue for ROXY user guide ed 2 Data can be presented as extracted ion chromatogram figure 11 of desired m z ratio value in case of amodiaquine m z of 356 354 326 and 299 are traced With help of the figure 11 where ElCs are presented it is easy to estimate the potential range in which the desired metabolite will have the highest abun dance E g for metabolite at m z 354 the best will be potential 300 400 mV however to form the metabolites 326 and 299 the higher value of potential 1200 mV should be applied To execute the program for 2 D Voltammogram 1 Go to pull down menu File gt Open Events and choose the program e g 2D_MS_Voltammogram_100_2000mV for GC electrode 2 Goto Events tab and press Start Using DC mode for the sample
3. MS start stop 1st MS start stop i i 100mV 0 1 51 1 96 2 01 2 46 11 51 11 96 Time min 0 50 1 00 1 50 2 00 10 00 10 50 Fig 10 Operation principle of mass voltammogram acquisition MS mass spectrometer Red labeled time indicates the potential change black labeled time corresponds to beginning and end of the MS acquisition Details see text To execute the program for 3 D Voltammogram 1 Go to pull down menu File gt Open Events and choose the program e g 3D_MS_Voltammogram_100_2000mV for GC electrode 2 Goto events tab and press Start CHAPTER 4 Events programming 15 2 D MS Voltammogram Additionally 2 D MS Voltammogram can be recorded and the data can be saved in one MS file as presented in the figure 11 This plot can be quickly generated with data analysis software of any MS Intens x1 EIC m z 356 EIC m z 354 4 EIC m z 326 EIC m z 299 o 4 2g a B67 Time min o 200 400 600 800 1000 1200 1400 E mv gt Fig 11 2 D MS Voltammogram of Amodiaquine The mass spectra are saved in one file for whole analysis EIC are representing the changes in oxidation of the Amodiaquine with respect to the potential applied Dialogue contains two additional programs that allow to acquire 2 D MS Vol tammograms 2D_MS_Voltammogram_100_2000mV and 2D_MS_Voltammo gram_100_3000mV The first event table is based on the program for the ac quisition of a mass voltammogram in the voltage range of 100
4. om ef 120 v Fiter off v He E 200mv Offset fo g Scan haf Data rate fio Hz Rate 50 v mV s Apply Autozero Read status 41115t 1115 0 Status default 32 Fig 7 Scan mode configuration window Pulse mode In the Pulse mode the potential follows a triple step block potential In contrast to the scan mode the pulse is applied immediately and continuously when switching on the cell In EC MS the pulse mode is used for example the regen eration of the electrode if the performance of the cell decrease without cell dis assembly Parameters in pulse mode Fig 8 e E1 measuring potential e E2 cleaning potential oxidative e 8 cleaning potential reductive e ts sampling time multiples of 20 ms e t1 delay sampling time e 2 time of oxidative cleaning step 0 2000 ms 10 ms steps e t3 time of reductive cleaning step 0 2000 ms 10 ms steps E2 E1 Fig 8 Operation principle of pulse mode 12 Dialogue for ROXY user guide ed 2 CHAPTER 4 Events programming A number of example event files is installed in the templates directory with the Dialogue software see Table 2 Table 2 List of the programs supplied with Dialogue Event name Description 3D_MS_Voltammogram_100_ 3 D MS Voltammogram for each potential 2000mV mass spectra are saved in separate data files Suitable for GC electrode 3D_MS_Voltammogram_100_ 3 D MS Voltamm
5. program Clean ing_Pulse_Mode_rev01 evt and can be executed automatically via events win dow The method can be found in My Documents and in the subfolders Dia logue Templates Note that to start pulsing using the Events program you need to change detection mode to Pulse first In case that no significant improvement of the cell performance is seen 1 For MD electrode use the additional procedure described the Chapter Maintenance Magic Diamond electrode of the relevant Cell user man ual 2 For GC electrode you can polish the electrode manually as described in the Polishing of the GC electrode chapter of the relevant Cell user manual Manual numbers 204 0010 u PrepCell and 201 7014 ReactorCell 22 Dialogue for ROXY user guide ed 2
6. Antec Dialogue for ROXY User guide 210 7017 Edition 2 2011 wl File Edit Tools Options Help Zc E Device settings cel 1 OOOO O DC Cell m Output Range 200 u FS Filter off v Hz Offset fo Z E cell 080 y 2 Data rate 10 Hz fos z ea KD a g z Read status 311154 1115 0 Status default Q 2 S lt Antec Industrieweg 12 2382 NV Zoeterwoude The Netherlands a T 31 71 5813333 F 31 71 5813334 E info myantec com W www myantec com M certified Q 9001 CHAPTER 1 Table of contents 1 Copyright 2011 Antec Leyden All rights reserved Contents of this publication may not be repro duced 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 ROXY Potentiostat DECADE I INTRO Sencell Flexcell Reactor ISAAC HyREF LINK ADF DECADE Dialogue ROXY Potentiostat Dialogue are trademarks of Antec Leyden BV Whatman 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 Data Apex are trademarks of DataApex Ltd Microsoft and Windows are trademarks of Mic
7. are Run the Dialogue software from Windows start menu under Antec Leyden software If a detector is connected it is automatically detected Otherwise the DEMO mode is activated See Help file for further details Log in password For first time users use the following name to log in Admin Exactly like this A uppercase No password required Connect ROXY trigger cable to the potentiostat and to MS to enable trigger MS acquisition MS should be in the remote mode and enable external trigger Contact your MS supplier for the details 6 Dialogue for ROXY user guide ed 2 CHAPTER 3 Dialogue Settings The Dialogue software controls both the ROXY EC System and the mass spec trometer start data acquisition the latter by means of an analog trigger con tact closure RELAY 1 The COM port settings of both the ROXY and syringe pump are configured in the Dialogue settings menu Fig 1 The ROXY poten tiostat will be connected automatically The syringe pump must be connected by user to the proper port if the port number is not listed the number can be ente red manually Once the devices are connected click fixed to avoid scanning all ports when starting Dialogue for the next time System Cell 1 Cell 2 Service Detector LC 100 110 3 38400 Dis Connect y 9600 Dis Connect I fixed Device found fixed ne Syringe pump 9600 vi Dis Connect fixed Fi
8. d Vista Dialogue is compatible with Windows 7 and Vista Since Windows Vista it is not possible to write data in the C Program Files Dialogue directory without chan ging security permissions Therefore all data is now stored in the common ap plications directory for Windows which is Win 7 amp Vista C ProgramData Dialogue Win XP C Documents and Settings All Users Application Data Dialogue Since Dialogue 201 786 Dialogue data amp templates are located in My Documents directory System requirements Requirements demo mode e PC with Windows 98 or higher incl NT 2000 XP Vista and 7 e Microsoft Excel 2000 or higher Requirements real mode e ROXY Potentiostat and syringe pump e PC with Windows 98 or higher incl NT 2000 XP Vista and 7 e free com ports for potentiostat and syringe pump e USB port for license dongle e Factory supplied serial cable regular serial cables don t work e Microsoft Excel 2000 or higher Installation e Run setup file to install the Dialogue software e Connect potentiostat and syringe pump with PC using factory supplied serial cables e Switch on devices CHAPTER 2 Installation guide 5 e Run Dialogue software from Start menu in Antec Leyden software e AFTER running Dialogue which installs dongle drivers insert the license dongle and restart software e f no detector is present Dialogue software will continue running in demo mode Running Dialogue softw
9. ed with the example of event program for the acquisition of conjugation experi ment The program run time is 15 10 minutes in total The acquisition of mass spectrum start after 5 0 minute delay and will contain data for Cell OFF Subsequently for 5 minutes the mass spectra are collected with the Cell at an applied potential of 800mV the value is set is program and can be adjusted All mass spectra are stored in one file Using scan mode to create MS Voltammograms Scan mode can be used for sample oxidation and for creating the MS Voltam mograms Continuous infusion of analyte FIA through the ReactorCell is used in combination with continuous scanning of potential The resulting oxidation products are measured in MS The E1 and E2 must be specify in the range the MS Voltammogram will be acquired Set the scan rate to desired value e g 10mV s Set the scan type to half and start the run the data will be saved in excel document 18 Intens Dialogue for ROXY user guide ed 2 Set the wide potential window e g set E1 to 0 V and E2 to 2 V for GC elec trode Turn ON cell Go to Options gt Start run Excel file will be saved Calculate the dead volume between ReactorCell and the ionization source of the mass spectrometer and recalculate the potentials to corresponding analy sis time points Fig 7 Estimate the potential value where the best results were obtained and desired product was formed with the highest yield follo
10. g 1 Dialogue settings window Options Settings gt RS232 The ROXY Potentiostat control When ROXY Potentiostat and syringe pump are connected it is possible to apply desired settings to ReactorCell or u PrepCell and syringe pump Main window of Dialogue Fig 2 open access to Cell 1 Cell 2 Devices Events and Data tabs All parameters can be set manually in the designated tabs or by programming them in the Events tab CHAPTER 3 Dialogue 7 File Edit Tools Options Help F Device settings cell 1 Data Monitor Devices Events r DC ji Output Range 00u Fiter ot Offset 0 Data rate fio Read status ps pms Fig 2 Dialogue main window Cell control tab in the DC mode Cell control Most important parameter for EC MS measurements is the cell on off selector and the potential setting Parameters are set in the Cell control window Fig 2 If data acquisition is used the range filter offset and run time can be set Out put range should be set to 200A It is default value since Dialogue 201 786 Devices In figure 3 the devices settings tab is shown In this window all relevant syringe pump settings can be configured such as syringe volume syringe diameter flow rate and flow direction infuse withdraw By means of the start stop but tons the pump can be activated with the configured settings
11. lable programs and details about MS Voltammograms acquisition are described in the further sections of this user guide r 5 ROXY Dialogue File Edit Tools Options Help Data Celli Cell2 Devices Events 2D_MS_Voltammogram_100_3000m _rev01 evt time min parameter value dev cell id comment Sort il 0 00 Syr Flow Rate 10 uL min Syr Pump This program is using the potential Add row 2 0 00 Cell on off off 00001 100 3000m Delsiw iow 3 0 00 Syr Pump Start infuse Syr Pump range for Magic Diamond electrod T lear 4 0 45 Ecell DC 0 10 00001 In case of use GC WE the potenti 5 0 50 Cell on off on 00001 should be adjusted to lower value Start 6 1 00 Ecell DC 0 20 00001 status Output A cf 1 50 Ecell DC 0 30 00001 Dead volume 15uL 8 1 51 Output relay 1 00001 TR ts 0 g 1 55 Output A inactive 00001 lll eei Start stop with run 3113E 113E 3 4 Status default 32 cell present 1K ADC 8 Max 2 5 m DD K Fig 4 Dialogue Events window CHAPTER 3 Dialogue Table 1 Commands used in events programming Parameter Value Description Syr Flow Rate 0 1 1000uL min Setting the flow rate of the syringe pump Syr Pump Start Stop Start Stop of the syringe pump Cell on off ON OFF Turn on off of the Cell Ecell DC 4 9 4 9V Applying voltage on the Cell Output A relay1 Starting run on the MS Output A Inactive Switchi
12. ncluding the measurement with the Cell off 14 Dialogue for ROXY user guide ed 2 The first acquisition of a mass spectrum starts after 1 5 minute delay and will contain data for the Cell off The delay is calculated based on the following pa rameters delay time gt V F e The dead volume Vg between ReactorCell and the ion source of the mass spectrometer For p n 180 0219 ROXY outlet assembly 2 MS this volume is 12 7 uL 1 meter red PEEK tubing ID 127um see reference 1 e The flow rate F of the syringe infusion pump in this case is 10 L min A slightly longer delay time is taken than based on the calculation to compen sate for the tolerance in tubing inner diameter affects volume and dilution in the tubing Poiseuille flow profile The dalay time depends on the tubing type and length dead volume and flow rate Calculate the delay time when different than supplied tubing is used or the flow rate is changed Adjust the programms if required The start of the mass spectrometer run is triggered by means of RELAY 1 The run duration is set to 0 45 minutes in the mass spectrometer data acquisition software and each MS analysis will stop after 0 45min MS analysis time was set to 0 45min in the MS software The operation principle is shown graphically in the figure 10 2000mV A Syringe pump End events start 400mV stop astm top 300mV 21st MS stare S gt j 2000mV al E 2 5 Q 2nd
13. ng relay off for next trigger signal Scan E1 2 rate 0 00 1 00 20 c Set the scan parameters coma separated E1 E2 type scan rate 1 2 5 10 20 50mV s scan type h alf f ull c ontinuous Scan ON OFF Start Stop Start Stop of the scan Pulse E1 3 t1 3 ts 2 00 2 00 0 00 Set the pulse parameters coma separated E1 300 200 200 20 E2 E3 t1 t2 t3 0 2000ms ts multiple of 20 ms EC Conditions Current from file Load the currently used EC conditions or saved in file range EC Operational modes Three operational modes are available DC pulse and scan and can be set in Select mode after acknowledgement by OK Changing mode will set the cell to off and all operational parameters are queried 7 Select mode cell 1 Cancel OK Fig 5 Select mode window Options gt Detection mode DC mode In DC mode a constant potential is applied It can be used in EC MS for MS Voltammograms recording and potential optimization as well as for continuous synthesis of specific metabolites with the highest yield Changing parameters in DC mode will have immediate effect unless an Apply button is present Cell and Acquisition parameters Cell potential E in DC mode and status Cell can be set and confirmed Ap ply The cell current is queried every second If the current is in overload a message appears If cell is off background c
14. ntage of scan over the DC mode is that the electrode surface is being regenerated du ring scanning and the cleaning of the electrode is required on the less frequent base Additionally using the scan mode it is possible to generate the set of metabolites that are formed within the scanned range however higher metabo lites yield can be achieved for some of the compounds in the DC mode Figure 15 shows the example of scanning experiment 10uM of Amodiaquine was scanned in range of 300 1200mV V since the optimal potential for formation of the metabolite at m z of 354 was 300mV and metabolites at m z of 326 and 299 the potential was 1100 and 1200mV respectively It is clearly seen that metabolite 354 can be formed at higest yield when DC potential of 300 mV was applied however in scan mode all metabolites are detected In the DC mode the metabolite 354 is not seen at higher potentials See Fig 6 20 Dialogue for ROXY user guide ed 2 0 E LLE 2 ESEO S S n a O E E ww 0 0 0 5 1 0 1 5 2 0 Time min m z 356 m z 354 m z 326 m z 299 Scan 300 1200 mV continuous Fig 15 Scanning for sample oxidation Amodiaquine E1 300 mV E2 1200 mV scan rate was 50 A s continuous It is possible to program scanning in the Events table Using pulse mode to clean the electrode This cleaning procedure is suitable for both MD and GC electrodes Refill the syringe with the mobile phase co
15. ntaining the supporting elec trolyte e g the same mobile phase used for oxidation of the sample and start the flow rate 20 50uL min Go to the Options pull down menu and choose Detection mode Select Pulse mode and click OK Set the parameters in the cell control window Fig 19 Table 3 It is recommended to set the Output Range to 200 UA Set Run time value to 5 min and turn on the cell Go to Options pull down menu and click Start Run Fig 20 Program will ask to save the data The excel file will be created And start the acquisition After the cleaning procedure turn OFF the cell and leave the flow for additional 1 2min Table 3 Cleaning pulse parameters CHAPTER 4 Events programming 21 Parameter Value E1 2V E2 2V E3 oV ti 1000 ms t2 1000 ms t3 0 ms ts 20 ms Output range 200A File Edit Tools Options Help Data Monitor Devices Events J Device settings cell 1 _ _ Pulse Output Pulse settings EC Mode Icell Range 200u4 FS E1 2 00 oott 1000 ms E cell 2 00 7000 Panga Fiter of Hz lee vo ms Fiter R E3 0 00 v Bjo ms Offset 0 v Offset ts 20 ms V out Datarate 10 Hz ewe E aux Cellon Autozero IV 1 t_pulse Read status 1 Status default 32 Fig 16 The cell settings in the pulse mode for MD electrode cleaning The cleaning procedure is available also as a
16. ogram for each potential 3000mV mass spectra are saved in separate data files Suitable for MD electrode 2D_MS_Voltammogram_100_ 2 D MS Voltammogram the data are 2000mV saved in one file Suitable for GC elec trode 2D_MS_Voltammogram_100_ 2 D MS Voltammogram the data are 3000mV saved in one file Suitable for MD elec trode Phase2 Method used for oxidation of the sample at 800mV and conjugation of the oxidation products with another compound Cleaning_pulse_mode Program for the electrochemical cleaning of the electrode Applicable for MD and GC electrodes Note that the supplied programs are exemplary and may need further optimization Using DC mode to create MS Voltammograms An MS Voltammogram is obtained using a syringe pump with continuous infu sion of analyte FIA through the ReactorCell to the MS The potential is incre mented in a couple of steps and mass spectra are collected Event files are available to automate this procedure The Dialogue controls the syringe pump the potentiostat and triggers the acquisition of mass spectra at CHAPTER 4 Events programming 13 the designated cell potentials A three dimensional MS voltammogram Fig 9 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 electrochemical generation of the desired metabolite for further resea
17. olour is orange E aux is potential measured on auxiliary electrode and is usually 50 500 mV different from E cell 10 Dialogue for ROXY user guide ed 2 Auto zero will set the output V out to zero or off set voltage Selecting Auto zero off releases the offset voltage Fig 2 shows the cell control window in DC mode Scan mode In the scan mode after starting a scan the potential is ramped between two extremes E1 E2 In the resting state E1 is applied Before starting the scan speed is set and the type of scan half full or continuous In EC MS the scan mode is used for fast MS Voltammogram acquisition less than 3 min is possi ble and for continuous metabolite synthesis or compound oxidation with range of potentials what can result in the set of metabolites formation In the figure 6 the scan mode is explained E2 Rate 20 mV sec 0 0 t s Half cycle Full cycle Fig 6 Operation principle of scan mode Parameters e E1 scan starting potential e E2 scan maximum potential e Rate scan rate 1 50 mV s e Scan scan cycle half full or continuous e If a half or full scan starts the Acquisition time is adjusted automatically e To start the scanning go to Options gt Start run CHAPTER 3 Dialogue 11 File Edit Tools Options Help Data i Monitor Devices Events F Device settings cell 1 r Scan m Output r Scan settings Range 200uA x Fs erf
18. oxidation Phase 1 Phase metabolites are oxidation reaction products of drug candidates Con tinuous infusion of analyte FIA through the ReactorCell is used to mimick the Cytochrome P450 reaction in the liver After estimating the potential using MS Voltammogram the sample can be oxi dized in DC mode by applying the optimal potential The simplest way is just to set the value in the cell control window and click Apply Figure 12 shows the example of applying different potentials in the DC mode The potential was applied as follow 1 Cell OFF no metabolites observed 2 300mV metabolite at m z of 354 3 1200mV metabolites at m z of 299 and 326 4 Cell OFF no metabolites observed Metabolite at m z of 354 was observed in solution with cell OFF but applying the potential shows Clearly its abundance increase CHAPTER 4 Events programming 17 m z 354 m z 326 m z 299 1200mV 0 2 lt 6 8 10 12 Time min Fig 12 Example of sample oxidation in DC mode The potential changes can be automated by programming the desired steps in the events tab Using DC mode for the sample oxidation and conjugation Phase I Phase II metabolite studies are based on conjugation of oxidation products with a substrate molecule such as glutathione for example In the conjugation experiments phase II the adduct formation of reactive me tabolite s with reagents like glutathione can be analyzed Dialogue is suppli
19. rch e g NMR Furthermore the 2 D version of MS Voltammogram can be recorded and the data can be saved in one MS file as presented in the fig ure 11 This plot can be quickly generated with any of MS software 3 D MS Voltammogram In the figure 9 the 3 D MS voltammogram of amodiaquine is shown To oxi dized Amodiaquine was oxidized with 400mV to its dehydrogenated metabolite m z 354 To form the other two metabolites m z 299 and 326 the higher po tential was required 1200mV For each cell potential mass spectra are re corded and saved in separate data files It simplifies data handling and the con struction of the MS Voltammogram N w A Intensity x10 4 1200 1000 T S s gQ 270 300 330 360 Ka m z Fig 9 3 D MS Voltammogram of Amodiaquine The plot is reconstructed from the separate mass spectra saved for each potential value The plot was made using Origin To acquire data for 3 D Voltammogram the supplied event program can be used e g 3D_MS_Voltammogram_100_2000mV or 3D_MS_Voltammogram _100_ 3000mV The programs start with the measurement with switching on the Cell and sub sequently the Cell potential is ramped from 100 2000 mV or 3000mV with incremental steps of 100 mV every 0 5 minute For each cell potential mass spectra are recorded for 0 45 minute and saved in separate data files 21 files or 31 files respectively in total i
20. ro gram The software package contains a set of event table files evt for the automa ted recording of mass voltammograms and parametric control of the events detection mode potential flow rate etc The set of pre programmed event tables can be used as a starting point for your own research and can be easily modified to suit your specific needs This document provides detailed background information about the supplied event table files and relevant Dialo gue settings Dialogue is a tool for e controlling all operational parameters incl syringe pump e programming timed events in one run or sequence e scanning voltammetry e potentiostat firmware upgrades using the FW upgrade wizard e creating and transmitting time files e PQ measurements e noise measurement There are no tools for further data analysis therefore Dialogue cannot be con sidered as fully featured chromatography software package The free demo version of this program has already functionality implemented The free version for the SDC is used for e firmware upgrades using the FW upgrade wizard e controlling all operational parameters e controlling IO ports for external devices e creating transmitting and running time files e control of the LC 100 HPLC pump isocratic mode 4 Dialogue for ROXY user guide ed 2 CHAPTER 2 Installation guide IMPORTANT You must have ADMINISTRATOR rights to install Dialogue and the USB drivers Windows 7 an
21. rosoft Corporation The information provided herein is believed to be reliable Antec Leyden shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing performance or use of this manual All use of the hardware or software shall be entirely at the user s own risk 2 Dialogue for ROXY user guide ed 2 Table of contents Table of contents 2 Dialogue for ROXY EC system 3 Installation guide 4 System requirements 4 Installation 4 Running Dialogue software 5 Dialogue 6 Seitings 6 The ROXY Potentiostat control 6 Cell control 7 Devices 7 Events 8 Operational modes 9 DC mode 9 Scan mode 10 Pulse mode 11 Events programming 12 Using DC mode to create MS Voltammograms 12 3 D MS Voltammogram 13 2 D MS Voltammogram 15 Using DC mode for the sample oxidation Phase I 16 Using DC mode for the sample oxidation and conjugation Phase Il 17 Using scan mode to create MS Voltammograms 17 Using scan mode for the sample oxidation 19 Using pulse mode to clean the electrode 20 CHAPTER 1 Dialogue for ROXY EC system CHAPTER 1 Dialogue for ROXY EC system The ROXY EC system is delivered with Dialogue software for ROXY p n 210 9005 Dialogue for Windows is a multi functional program to control the DECADE II electrochemical detector and ROXY potentiostat It runs simultane ously with Windows compatible integration software or any other Windows p
22. w the EIC of the m z ratio of the selected compound Fig 8 Check neighbouring potentials if the estimation made in point 5 was accurate E g from figure 7 the optimal potential is between 1050 mV to 1250 mV 1100 mV was chosen to further tests but also 1200 mV and 1000mV were checked Use the potential established in points 5 and 6 to oxidize the sample to give the desired products in DC mode or range of potential in the scan mode for details how to use the scan mode for compound oxidation see further section of this user manual xd m z 356 m z 354 m z 326 oe m z 299 m z 370 0 5 1 0 1 5 2 0 2 5 3 0 Time min eee Startscan 300 600 900 1200 1500 E mV Fig 13 Scanning voltammetry of 10 umol amodiaquine at a glassy carbon working electrode at a scan speed of 10 mV s and E1 0 and E2 1500mvV The m z ratios of different metabolites of Amodiaquine are plotted see legend CHAPTER 4 Events programming 19 Intens m z 326 ereere 0 5 1 0 1 5 2 0 2 4 3 0 Time min a S S F oo Startscan 300 600 900 1200 1500 E mV Fig 14 Scanning voltammetry of 10 umol l amodiaquine at a glassy carbon working electrode at a scan speed of 10 mV s and E1 0 and E2 1500mV The m z of 326 is plotted The shadow area shows the optimum potential range 1050 1250mV Using scan mode for the sample oxidation The scan mode can be used for efficient sample oxidation The adva
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