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EC301 Manual - Stanford Research Systems

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1. Program Program E I CE voltage AD measurement L KE CEADC measurement Local feedback bandwidth control Compliance limits a CE 5 IS 3 gt AY O oo y L E Error Voltage ae amplifier clamp Cell CE sense Potentiostat j j Current interrupt Front panel 6 4 galvanostat cell switch safety switch Difference or ZRA mode J5 000 amplifiers WE sense WE Current gt to gt voltage OO o Voltage Bias rejection Anti alias measurement 10 Hz lowpass O E output O front panel owpass A O Raw E output rear panel mo hae Current Bias rejection Anti alias measurement 10 Hz lowpass O output O front panel owpass y 3 Raw output rear panel Figure 1 EC301 block diagram 2 EC301 basics 2 3 Polarity convention 2 3 Polarity convention The relative polarity of voltages and currents handled by the EC301 follows the American polarity convention As illustrated in Fig 2 this convention calls for cathodic reducing currents to be taken as positive Voltages are programmed taking RE as the reference potential so asking for 1V with the external input or the front panel will move the WE potential 1V above RE We invert the polarity of the front and rear panel VOLTAGE outputs relative to the front panel di
2. A 1 1 1 1 1 1 v 1 byte 1 byte 2 bytes 4 bytes 4 bytes 1 byte 1 byte 2 bytes 4 bytes 4 bytes 4 bytes 4 bytes 1 byte 6 bytes 1 byte Figure 28 Basic construction of the data packet used for streaming data The four bytes of fast instrument state in each data frame are described in table 4 on page 84 The E I overload record byte in the footer is described in table 5 on page 85 S RS Stanford Research Systems 83 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 0 On closed 1 Off open Power line synchronization toggle Toggle after each zero crossing Cell switch position O Not limiting li limiting status ee Compliance limiting status 1 Limiting Current I range OANDOKWN HEH E o 0 Voltage E range 1 Running Ramp waveform synchronization toggle Toggle after ramps begin and repeat 15 18 Data averaging window width N 2N points wide 0 Idle 1 Running Pulse waveform edge toggle Toggle after each edge Pulse waveform synchronization toggle L ae begr Ramp waveform generator status tle 1 1 2 Pulse waveform generator status 0 Idle Arbitrary waveform generator status i Reading Toggle after arbitrary waveforms begin Arbitrary waveform synchronization toggle And sepia Table 4 Fast instrument state bitfields built into each data frame SRS stanford Research Systems 84 EC301 Potentiosta
3. SRS stanford Research Systems 26 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 1 Front panel 3 1 12 IR compensation IR compensation involves adding an extra voltage to the control program voltage to compensate for drops between RE and WE Use the MODE key to toggle between two ways of generating this O INTERRUPT voltage positive feedback and current interrupt Compensation will not be applied until the ENABLE key is pressed IR COMPENSATION ENABLE FEEDBACK INTERRUPT mode Figure 6 illustrates the parameters used for cur MODE SET rent interrupt when engaged from the front panel In this mode the CE is periodically disconnected from the control electronics to interrupt the cell current This removes any IR drop between the reference and working electrodes causing Vwr sense Vre to drop by AV The EC301 then takes two samples of Vwe sense Vre to measure this drop one after interruption and one after control is restored This value along with the percent correction factor is used to calculate the boost potential AV added to the program voltage Vwe sense Vre Second interruption cycle A gt Time Figure 6 Cell potentials during current interrupt IR compensation Default values for the various parameters are shown in table 1 Use the SET key in INTERRUPT mode to adjust the percent correction factor the only parameter than can be set from the front panel The o
4. 2000 Galvanostat Hens 000 1999 1998 2000 1_1000 gt 1000 for 1A range The i parameter chooses the control point to set or query The point values take mV values in potentiostat mode and milli fractions of the full scale current range in galvanostat mode As illustrated in figure 31 these values can be added to the baseline to form the finished waveform For example the command pdatap O 1000 sets the value of Po to 1V in potentiostat mode or range in galvanostat mode SRS stanford Research Systems 101 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name pholdt Set or query the pulse data waveform control point hold times Description Each of the possible six control points used to specify a pulsed waveform needs a hold time Range 0 1 2 5 Units Range holdt il x p an x 1 2 3 16777215 24 1 The i parameter chooses the control point to set or query Figure 31 shows hold times To and T for points Py and P For example the command pholdt 0 2000 sets the To hold time to 8ms SRS stanford Research Systems 102 EC301 Potentiostat Galvanostat ZRA 7 Remote programming pincrm i j k 7 3 Detailed command list Name pincrm Configure how a pulsed waveform point interacts with the baseline Description Each control point in the pulsed waveform can either add its value to the baseline or to OV 0A to form the
5. 7 3 Detailed command list 7 3 15 Status reporting commands ESR i Name ESR Query the Standard Event Status register Description This command returns values from the Standard Event Status reg ister Sending ESR will return the entire register value in decimal format while sending ESR i will only return bit i Reading the register will also clear it Sending ESR will clear the entire register while sending ESR i will only clear bit i Table 6 below lists the conditions corresponding to the register bits Use the ESE register described on the following page to enable these bits to set a bit in the Status Byte See figure 29 on page 99 for an overview of status bit promotion Bit Name Pssst when SES when Bit Name sSetwhen A The OPC command has completed ae Query error data has been lost instead of transmitted Device specific error an error was encountered while executing a remote command Execution error a remote command could not be executed due to an argument or state problem Command error an invalid remote command was received User request front panel activity was attempted regardless URQ of local remote status The unit has turned on Table 6 The Standard Event Status register bits The Standard Event Status register is defined by the TEEE 488 2 1987 standard and is used primarily to report errors in commands received over the remote interface These b
6. SRS stanford Research Systems 74 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 8 Analog output commands Name brenab Set or query the use of bias rejection Description The EC301 uses bias rejection to remove DC voltages from the front panel VOLTAGE and CURRENT outputs 0 Bias rejection disabled Automatic bias rejection Sending brenab 1 begins automatic bias rejection by triggering a measurement of the front panel VOLTAGE and CURRENT signals This is a simple detection of the constant component bias of these signals Once this bias is detected the EC301 attempts to null reject it by adding constant voltages to the BNC outputs Custom bias rejection amounts can be entered with the bireje command described on page 75 and the bireji command described on page 76 Note that you can only use these commands after sending brenab 1 to turn bias rejection on brenab i Example setvol 1000 Programs a 1V controlled voltage in potentiostat mode ceenab 1 Closes the cell switch to engage control brenab 1 Begins automatic bias rejection brenab Is bias rejection enabled 1 Yes it is bireje What is the nulling voltage applied to VOLTAGE 998 Automatically applied value in mV bireje 1000 Send a custom nulling value for the VOLTAGE output bireje What is the nulling voltage applied to VOLTAGE 1000 bireji What is the nulling voltage applied to CURRENT 0 87 Automa
7. This command can still be used to indicate when the instrument is ready to process new commands In this example DPC Long process finishes 1 waiting for the 1 to be returned would indicate completion of all commands The non query version of the command simply sets the OPC bit in the Standard Event Status Register when the long process finishes See the ESR documentation on page 90 for a description of this register Name WAI Wait to continue Description This command is implemented for compatibility with the IEEE 488 standard The original intent was for WAI to prevent the instrument from executing commands until it completed all pending operations SRS stanford Research Systems 86 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name verbmd Set or query the instrument s verbosity Description This command sets or queries the instrument s verbosity using the mapping below In terse mode the instrument will issue no unsolicited output such as error messages This mode suits automated equipment that can not handle unexpected inputs In verbose mode the instrument will issue warning and error ayia verda messages as needed 1 Verbose mode Name lockfp Set or query front panel lockout Description The front panel keypad can be disabled to prevent inadvertent adjustments ETT dd 0 Front panel unlocked normal operation Front panel disabl
8. This output allows triggering an oscilloscope or synchronizing other data acquisition using with the start of a scan As illustrated in SCAN SYNC figure 9 this output is brought low immediately before the scan begins and before every scan repetition during continuous scans The output is held low for 10 us before returning high which limits the rate to roughly 50kHz The EC301 can not reliably send trigger OUTPUT pulses for repetition rates faster than this A High 10us lt gt Scan sync output lt Ius lt Low Program E I gt Time Figure 9 The SCAN SYNC output is brought low at the beginning of a scan and held there for 10 ps SRS stanford Research Systems 37 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel 3 2 9 Auxiliary ADC inputs 1 3 These 10 V inputs allow monitoring analog signals like flow rate ADC 1 ADC 2 ADC 3 pH or temperature along with E and I data Using the remote interface data from these inputs can be synchronized with E and I collection to within 1 ms Use the synchronous ADC input de scribed in section 3 2 14 on page 43 for tighter timing requirements INPUT INPUT INPUT Use the getaux command described on page 80 to acquire data from these BNCs using the remote interface SRS stanford Research Systems 38 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel 3 2 10 Resistance temperature detector RTD input Th
9. adjusting values using the knob Times are adjusted using the knob for individual fields and the arrow keys described in section 3 1 16 on page 30 to move between the fields shown below 00 00 00 0000 Wr ae oe hours minutes seconds seconds 10 The maximum hold time for a LSV is 99 59 59 9999 100 us short of 100 hours The setability is in 100 us steps Choose the scan end condition Figure 20 a illustrates the cell potential for the E end condition while 20 b shows it for OPEN CIRCUIT If the end condition is OPEN CIRCUIT the cell potential will be free to drift after the T wait time If the condition is FE the potential will immediately return to E Choose SINGLE or CONTINUOUS scanning Single scans illustrated in figures 20 a and b go to the end scan condition after the T gt wait time Continuous scans illustrated in figure 20 c track back to F after the T wait time with the same rate used for the forward ramp They then repeat the entire program indefinitely Choose the trigger mode MANUAL allows the GO ARM key to trigger the scan while EXTERNAL mode requires the rear panel scan trigger input See section 5 4 on page 61 for a better description of scan triggers in general and section 3 2 6 on page 34 for a description of the rear panel scan trigger SRS stanford Research Systems 52 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 1 Setting scan parameters potentiostat
10. galvanostat mode 5 2 1 Cyclic current ramp Figure 23 illustrates the parameters needed to specify a cyclic current ramp scan The procedure is as follows 1 Use the MODE key to select CV While this scan mode is named for its use in potentiostat mode it will set up a cyclic current ramp in galvanostat mode 2 Cycle through the required parameters using SET and adjust values using the knob 3 Choose the scan end condition Figure 23 a illustrates the cell current for the J end condition while 23 b shows it for OPEN CIRCUIT 4 Choose SINGLE or CONTINUOUS scanning Single scans illustrated in figures 23 a and b go to the end scan condition after reaching J on the return ramp Continuous scans illustrated in figure 23 c immediately turn around to repeat the forward ramp and then the entire triangle shaped waveform 5 Choose the trigger mode MANUAL allows the GO ARM key to trigger the scan while EXTERNAL mode requires the rear panel scan trigger input See section 5 4 on page 61 for a better description of scan triggers in general and section 3 2 6 on page 34 for a description of the rear panel scan trigger gt gt Time Time a A cyclic current ramp program using SINGLE scan b A cyclic current ramp program followed by a simu type and J end condition lated jump to open circuit zero current using SINGLE scan type and OPEN CIRCUIT end condition The cell current and potential are uncont
11. ground LL b One of many undesired current flow paths with floating and signal ground posts connected Figure 18 Disconnecting the signal and floating ground terminals on the EC301 allows current to flow in circuits including earth ground SRS stanford Research Systems 49 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 5 1 5 1 Performing scans using the front panel Setting scan parameters potentiostat mode 1 Cyclic voltammetry CV Figure 19 illustrates the parameters needed to specify a CV scan The procedure is as follows 1 2 Use the MODE key to select CV Cycle through the required parameters using SET adjusting values using the knob Times are adjusted using the knob for individual fields and the arrow keys described in section 3 1 16 on page 30 to move between the fields shown below 00 00 00 0000 o e hours minutes seconds seconds 10 The maximum hold time for a CV is 99 59 59 9999 100 us short of 100 hours The setability is in 100 us steps Choose the scan end condition Figure 19 a illustrates the cell potential for the Ej end condition while 19 b shows it for OPEN CIRCUIT Choose SINGLE or CONTINUOUS scanning Single scans illustrated in figures 19 a and b go to the end scan condition after reaching E on the return ramp Continuous scans illustrated in figure 19 c immediately turn around to repeat the forward ramp and then the ent
12. vfdmsg 0 string to display will print STRING_TO_DISPLAY on the top line of the character display Name nulcmd Do absolutely nothing Description This command is useful for testing the remote interface without doing any harm Sending the nulcmd query will always return 0 Example nulcmd Does nothing but write O to the transmit queue 0 SRS stanford Research Systems 88 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 14 Timebase commands Name exttmb Query the timebase Description This query only command returns the state of the sampling time base io Timebasesetting__ io Timebasesetting__ E Internally generated no external timebase present exttmb i Externally generated external timebase automatically selected when present Internally generated external timebase present but disabled via the autotb command described on this page Name autotb Turn automatic timebase selection on or off Description This set only command turns automatic timebase selection on or off Use the exttmb query described above to query the timebase selection state Manual mode timebase generated internally even though an external timebase is present autotb i Automatic mode timebase generated internally by default but accepted from external source if present SRS stanford Research Systems 89 EC301 Potentiostat Galvanostat ZRA 7 Remote programming
13. GALVANOSTAT ZRA TRACKING STANFORD RESEARCH SYSTEMS MEASUREMENT SETUP CONTROL CONFIGURE AN GPIB Tcpip DISPLAY CURRENT RANGE IR COMPENSATION INTERRUPT ev e_ iw O_ step O oren aRcuT 0 5 scan ENDSAT ia are O FeeDeAcK O 100ma O toma ee eS L MODE J 10Hz 3 LOWPASS n m FILTER ROTATING ELECTRODE d A 30V 1A MAX COMPLIANCE VOLTAGE CURRENT 502 OUTPUTS LOAD WITH 10k0 3 1 1 Power on reset REMOTE STATUS ASRS O sro O ACTIVITY REMOTE MODE ERROR EXT TIMEBASE RS Stanford Research Systems O since Es continuous EXTERNAL INPUT O im O 100 na O ona ina REMOTE STATUS PS o os e 7 o ME O E so 530 SCAN conmroL HOLD A o rre OZ k GO ARM PAUSE actvny gt d How Ei l ll O EXTERNAL d O REMOTE MODE manual TRIGGER XX 100 08 a O tsvoramosr a O ona L 2 2VGALVANOSTAT Hooe E C A SETA ADVANCE STOP GJS ERROR O EXTTIMEBASE ASRS O im 10KO 50 pF SIGNAL GROUND To restore the instrument to its factory default settings from the front panel hold down the LOCAL key while the power is turned on 21 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 1 2 Bandwidth limit BANDWIDTH LIMIT 3 1 3 CE limit CE LIMIT LIMITING 3 1 4 Cell ENABLE A 30V 1A MAX
14. arbtyp i 7 3 Detailed command list Name arbget Query the value of the arbitrary waveform at index i Description To determine what value is programmed at any index use arbget If no value is programmed at the given index i arbget returns an error code 31 Name arbtyp Set or query the arbitrary waveform type Description The user must set the arbitrary waveform type with arbtype before entering data points with arbset The arbtype command argument defines the legal range of arbset arguments This waveform type can only be defined once This prevents mixing control point data types in memory This also means that the arbrst command must be sent between arbtyp commands CO Potentiostatic 15V 1004A Galvanostatic Notice that there is a scan type for each current range Arbitrary waveform points for galvanostat scan types are simply fractions of the full scale current so there must be a way to define this current After setting a galvanostatic scan type sending arbrun 1 or arbrun 2 will force the instrument into the range defined by the scan type SRS Stanford Research Systems 114 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name arbrun Begin end or arm arbitrary waveform playback Description This set only command allows for either internal or external trig gering of arbitrary waveform scans EN Instruction disarm the scan to ignore SCA
15. armed state See section 3 1 14 on page 29 for more information about the external trigger setting See trgarm i section 3 2 6 on page 34 for more information about the rear panel scan trigger input O Unamed Armed waiting for extemal scan tigger Armed waiting for external scan trigger Name scntrg Query the scan trigger state are we scanning Description This command will tell you if the instrument is running an auto matic scan scntrg Not triggered Triggered scanning Name stsync Set or query whether software triggered scans are synchro nized with the power line cycle Description If the argument to STSYNC is 1 a remote command software triggered scan i e not triggered from the front panel will not begin until the power line cycle measuring circuit detects a zero crossing This allows the user to synchronize a fast cyclic voltammogram to occur at the same point in a power line cycle each time such a trigger is issued The default is not to gate with the power line cycle and begin the scan immediately 0 No power line synchronization Software triggered scans aligned to power line cycle stsync i SRS stanford Research Systems 73 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 7 Rotating working electrode commands Name rotate Set or query the rotator output voltage Description No description 010000 rotate x
16. gt Time Figure 36 Arbitrary waveform example Points are played back at the 1MHz arbdiv rate so use repeated values to get longer hold times Waveforms can have 1600 programmed points SRS stanford Research Systems 120 EC301 Potentiostat Galvanostat ZRA References References 1 A J Bard and L R Faulkner Electrochemical Methods Fundamentals and Applications John Wiley and Sons 1980 SRS stanford Research Systems 121 EC301 Potentiostat Galvanostat ZRA References A Measuring cell voltages at the cell The EC301 s WE connection must not be connected to an external instrument s ground when measuring cell voltages Doing so would divert cell current from the WE to the external ground and thus invalidate current measurements Figure 37 illustrates good and bad ways of making these measurements Figure 37a shows a high impedance differential preamplifier used to buffer the desired voltage before sending it to an oscilloscope Figure 37b shows a handheld meter used to make the measurement directly Figure 37c shows the ground pigtail of an oscilloscope probe incorrectly connected to the WE electrode diverting cell current away from the EC301 s measurement electronics and possibly destabilizing the cell The methods shown in figures 37a and 37b are correct because both probes in each case are floating not connected to ground The method shown in 37c is incorrect because the oscilloscope probe pigtail does not
17. 2 Setting scan parameters galvanostat mode o e 97 5 2 1 Cyclic current tamp s 2 a e e es eei ae e ode ba a a ea 57 5 2 2 Linear Current Tanpo da a e BE tdi ide Be et a 58 5 2 3 Current St ps a o Adeeb DD AA wee eee Po be ee Pa 59 5 2 4 Current Hold 4 2 4 0 Be eh a A BOO LE ee a 60 5 3 Basic scan Controls sorra sawek Boo bee GR ENM Be eee ead ad eS 61 De TIP PEMINE RI GP Be be eee Ee A 61 5 4 1 Triggering a scan from the front panel 2 2 ee 61 5 4 2 Triggering a scan with the scan trigger input 2 2 2 ee 61 5 4 3 Triggering a scan from the remote interface 2 0 a 61 5 5 Setting the end of scan condition e e 61 6 Using the EC301 with a frequency response analyzer FRA 63 7 Remote programming 64 EL Command Syntax cu la a be o A a A a da 64 7 2 Argument formats i664 sad ac a Ee ew a 64 Ta Detailed scommatid list s s eie pa cen Ghee Sd EE a SHOE a A 65 7 3 1 Firmware and hardware revisions 02 00 eee eee eee 65 7 3 2 Program E I setup with external input o o e e 65 7 3 3 Control loop commands e a a 4 4 4 22 45 ds eee A Ea A ee ee A ee E 68 7 3 4 Cell switch s a ssor ge he bbb badad ea beeu eee a ede G eam a R 70 7 3 5 IR compensatio N od e Bitte et ee A es As ee Be Sts E d 71 7 3 6 Scan trigger commands ss oe hee eR ES ER Ree ee ee Be a 73 7 3 7 Rotating working electrode commands 2 002000 000004 74
18. 3 1 Front panel 3 1 14 Measurement setup control MEASUREMENT SETUP CONTROL OPEN CIRCUIT O E SCAN ENDS AT O_ pate Pa SINGLE py Es l Oo HOLD 0 0 a CONTINUOUS 1 SCAN TYPE GO ARM PAUSE gt Il EXTERNAL MANUAL ADVANCE STOP gt gt TRIGGER A variety of automatic scans and holds can be programmed from the EC301 s front panel Once the scan type is selected you will be prompted for a set of necessary parameters When GO ARM is pressed with a MANUAL trigger setting the EC301 will engage control apply the scan and remove control as required by the scan end condition Use the MODE key to select a scan type These types are described in section 5 on page 50 Use the TRIGGER key to select the action of GO ARM In MANUAL mode the programmed scan will begin when GO ARM is pressed In EXTERNAL mode pressing GO ARM will arm the EC301 preparing it to scan with the next rising or falling edge received at the rear panel SCAN TRIGGER input This allows the scan to be triggered by other experimental events See section 3 2 6 on page 34 for more information about the SCAN TRIGGER input 3 1 15 Knob Use the knob to enter numbers via the character display The knob TRACKING is velocity sensitive so experiment with different rotation speeds to set large numbers The TRACKING indicator will light when turning the knob will immediately affect cell conditions For example if a hold
19. AC line voltage in AC POWER put and to block high frequency noise from entering or exiting the instrument 90 VAC to 260 VAC 47 Hz to 63 Hz 3 2 2 GPIB interface The 24 pin GPIB connector allows a computer to control the EC301 IEEE 488 via the GPIB IEEE 488 instrument bus The GPIB address is INTERFACE set with the front panel GPIB key SRS Stanford Research Systems 32 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel 3 2 3 Ethernet interface There are two LEDs on the RJ 45 ethernet connector The green ETHERNET LED lights only when the system is transmitting The yellow LED INTERFACE lights whenever it sees any packet on the wire This includes pack ets not destined for the EC301 i LI 3 2 4 Current interrupt synchronization This digital output allows triggering an oscilloscope or other data Cl acquisition at the beginning of current interruption This output SYNC will be brought low before just before interruption begins and re turned high after it ends The timing diagram is shown in figure tes OUTPUT A high Cl SYNC low I 1 I I closed CE switch lt Ius lt lt 118 I open interruption interruption begins ends Time Figure 7 Timing diagram for the CI SYNC digital output 3 2 5 Timebase synchronization input This BNC can accept a 10 MHz reference signal from an external source to improve the stability of the int
20. COMPLIANCE S RS Stanford Research Systems 3 1 Front panel Use the A and V keys to increase or decrease the control band width The counter electrode CE voltage relative to ground can be lim ited to protect sensitive cells Using the ENABLE key to enter the limiting mode allows reducing the maximum CE voltage from 500mV to 30 V This maximum is adjusted by pressing the SET LIMIT key and turning the knob The tracking light will indicate that the CE limit follows the knob movement The external electrometer should be connected to the main box using this DB 25 connector The umbilical should be securely fas tened to this connector using the jack screws on either side Use the ENABLE switch to manually disconnect the CE from the power amplifier whenever you must come in contact with the cell electrodes This switch is illuminated when the CE is connected to the control circuitry When this switch is in the instrument connects or disconnects the CE as needed When out the CE is always disconnected and the switch is dark 22 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 1 Front panel 3 1 5 External electrometer The external electrometer face contains the counter electrode CE output three electrometer inputs the working electrode WE cur rent input and a grounded binding post See section 4 for il pe ce a lustrations of how these inputs and outputs are used in different
21. IRENAB 1 Turn current interrupt on Vwe Volts vs reference OV Time Figure 35 Sample current interruption waveform SRS stanford Research Systems 119 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 4 Programming examples 7 4 4 Arbitrary waveform The following command sequence produces the waveform shown in figure 36 This arbitrary waveform example includes five ARBSET points and three cycles The scan ends with the system in control at the first data point ARBRST Reset the arbitrary waveform interface ARBTYP 1 Waveform data type will be potentiostatic ARBDLY 1 Hold Do for one second then play D ARBCYC 3 Cycle the waveform three times ARBEND 0 Maintain control at Do when finished ARBDIV 1000 Play points back at 1MHz 1000 1ms sample time ARBSET O 100 Set the Do point at 100mV 0 EC301 responds 0 ARBSET 1 200 Set the D point at 200mV 0 EC301 responds 0 ARBSET 2 500 Set the Da point at 500mV 0 EC301 responds 0 ARBSET 3 100 Set the D3 point at 100mV 0 EC301 responds 0 ARBSET 4 100 Set the D4 point at 100mV 0 EC301 responds 0 arbrun 1 Start the scan Repeating scan unit D 500mV 20 gt gt 1ms 8 S fa D Scan ends with 2 1 D 200mV control at the 2 D D D first D 9 point 3 100mV e gt lt gt gt p 1s 100mV 6 D D
22. SENSE SENSE e instrument modes SIGNAL WE GROUND CE counter electrode output This is the output of the EC301 s control amplifier It can source or sink 1A into a 30V to 30V range CE SENSE input This electrometer input is used with WE SENSE in ZRA mode to monitor the voltage between two typically identical electrodes As shown in figure 12 it is named for usually being connected to the CE output RE reference electrode input As illustrated in figure 1 this electrometer input is used with WE SENSE to monitor cell potentials WE SENSE input As illustrated in figure 1 this electrometer input is used with both the RE and CE SENSE electrodes to monitor cell potentials WE input This input connects to a shunt resistor used to measure current flowing in the working electrode The input resistance here will vary with the current range setting SIGNAL GROUND This can be connected to a Faraday cage to isolate sensitive cells from electrical noise 3 1 6 Voltage This display shows the results of the internal VwE sense VRE measurement The OVERLOAD light indicates when the cell potential exceeds 15 V relative to signal ground Measurement accuracy will degrade from specifications outside of this range VOLTAGE OVERLOAD 3 1 7 Current This display shows the results of the internal cell current mea surement The OVERLOAD light indicates when current exceeds 2 x Irange or 1A where
23. See section 7 3 8 on page 75 for the appropriate remote commands Neither changing the current range nor enabling autoranging is allowed while bias rejection is active SRS stanford Research Systems 25 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 1 Front panel 10 Hz LOW PASS FILTER Use this key to simultaneously filter both the VOLTAGE and CURRENT analog outputs The front panel filter has a 6 dB octave rolloff with a 3 dB frequency of 10 Hz You can customize filter settings using the lpfili and lpfile commands described in section 7 3 8 These commands allow filtering a single output instead of both Note that the 10 Hz LOW PASS FILTER key will light whenever filtering is applied to either output 3 1 11 Current range Use the A and V keys to select a current range A cell current SURRENT RANGE Iwg equal to the selected current range Iwg frange gives 1 V at the CURRENT output BNC Ignc 1 V Likewise 1 V applied ia to the EXTERNAL INPUT BNC in galvanostat mode will generate a O 100 ma controlled current of frange auna Currents exceeding 2X range or 1 A will generate an overload e condition While the EC301 can accept currents lt 1 A in any vuln range without damage measurement accuracy is degraded during vd we overloads ec Use the AUTO RANGE key to toggle automatic selection of O om Irange based on the measured cell current Note that auto ranging O in is not allowed in galvanostat mode
24. Systems 92 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name INSE set or query bits in the Instrument Status Enable Register Description The INSE i command sets the Instrument Status Enable register to the decimal value i 0 gt 65535 The INSE i j command sets bit i 0 15 to j 0 or 1 As shown in figure 29 on page 99 bits enabled in the INSR register defined on the preceding page via the INSE register this one set the INSW bit in the status byte The INSE query returns the value of the Instrument Status Enable register The INSE i command queries only bit i INSE 7 i j When the instrument sets a bit in the Instrument Status Register and the corresponding bit is set in the Instrument Status Enable register by the user bit 1 INSW of the Status Byte is set This causes a SRQ if bit 0 in the Status Byte Enable register is set Example INSE Returns the register value in decimal format INSE 2 Returns 0 if bit 2 is cleared or 1 if it is set INSE 16 Sets the register value to 16 bit 4 set INSE 4 0 Clears bit 4 SRS stanford Research Systems 93 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name MESR Query the Measurement Status register Description This command returns values from the Measurement Status regis ter Sending MESR will return the entire register value in decimal format while sending MESR i will o
25. WE e Output current 0 2 of current range all other ranges sense electrodes held within 5mV of each other 1A range 1 A min 1 A max All other ranges 2x full scale min 2X full scale max SRS stanford Research Systems 9 EC301 Potentiostat Galvanostat ZRA 1 General information 1 3 Specifications General control loop e Bandwidth control 10Hz 100Hz 1kHz 10kHz 100kHz gt 1MHz Bandwidth limits 10kQ resistive load lt 1004A output cur rent e Compliance limiting Cell current ICE Voltage limit accuracy 250mV HV SRS Stanford Research Systems 10 EC301 Potentiostat Galvanostat ZRA 1 General information IR compensation e Current interrupt Switching time on gt off Interrupt time Interrupt frequency e Positive feedback Range Resolution S RS Stanford Research Systems 1 3 Specifications lt 5us 1 KQ resistive load 100us gt Is 0 1 Hz gt 300 Hz 1m for 1A range 1MO for InA range EC301 Potentiostat Galvanostat ZRA 1 General information General system e Remote interfaces LAN 10 100 base T Ethernet GPIB IEEE 488 e Dimensions W x H x D Main box 17 x 18 5 x 5 25 inches External box 3 25 x 4 75 x 2 5 inches Umbilical 36 inches Weight Power e RTD measurement Temperature sensor User supplied 1002 Pt RTD a 0 00385 0 0 C Range 100 C to 200 C Resistance measurement accuracy 0 30 S RS Stanford Rese
26. and rate point indexes RAMPRS SCANTP SCANEM RAMPPT RAMPDT RAMPRT RAMPPT RAMPDT RAMPRT RAMPPT Initialize the ramp generator 1 Set single not continuous scan type 1 Set the scan endpoint to Eo O 100 Set the Ej point at 100mV 0 60000 Set the To delay time to 6s 0 2000 Set the Ry ramp rate to 0 2V s 1 1 1 2 500 Set the E point at 500mV O No delay at the E point 2000 Set the R ramp rate to 0 2V s 100 Set the E gt point at 100mV RAMPPG O Load the ramp program verify parameters RAMPST 0 5V Vwe Volts vs reference 0 1V O Start the scan 4 6s Time Figure 34 Sample cyclic voltammetry waveform SRS Stanford Research Systems 118 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 4 Programming examples 7 4 3 Current interrupt IR compensation This example doesn t completely set up IR compensation but it illustrates the use of the remote commands described in section 7 3 5 on page 71 Figure 35 below illustrates interruption of current through a resistor with no actual correction applied The commands below set up the timing parameters and start interruption IRTYPE O Set current interrupt mode CIOPEN 3000 Set the interruption time to 3ms CIPERD 10 Set the interruption period to 10ms CICORR O Set the correction amount in percent CIDLAY O 100 Set the open voltage sampling delay to 100us CIDLAY 1 100 Set the closed voltage sampling delay to 100us
27. flat blade screwdriver 4SRS Stanford Research Systems 19 EC301 Potentiostat Galvanostat ZRA 2 EC301 basics 2 4 Connecting the EC19 to the EC301 2 4 2 Steps 1 Identify the connection points on the EC19 There are two jack screws on the rear panel of the unit shown in Fig 4 Figure 4 EC19 rear panel connector Securing the umbilical cable 2 Screw the umbilical cable screws into the jack screws of the EC19 as shown in Fig 4 3 Identify the connection points on the EC301 There are two jack screws on the front panel of the unit shown in Fig 5 Figure 5 Front panel umbilical connector on EC301 Securing the umbilical cable to the EC301 4 Screw the umbilical cable screws into the jack screws of the EC301 as shown in Fig 5 5 Power up the EC301 switch is on rear panel If you get any front panel errors about the EC19 turn off the EC301 Check the umbilical connection on both ends and power up the EC301 again If errors persist contact SRS 4SRS Stanford Research Systems 20 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 Operation This manual will refer to a key with brackets such as Key 3 1 Front panel BANDWIDTH LIMIT CELIMIT VOLTAGE OVERLOAD i vz N iookz ENABLE 2 10K Ortiz O100Hz tore setumir gt o ANALOG OUTPUT LIMITING O PoTENTIOSTAT GALVANOSTAT O za ENABLE O camote CURRENT OVERLOAD EC301 POTENTIOSTAT
28. grammed pulsed waveform Name plstop Stop the pulsed waveform plstop Description This command halts the pulsed waveform leaving the control loop closed SRS stanford Research Systems 105 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 17 Ramp generation commands E I 4 E a batas Es 1z A siaiaetalatatatataionaetaientataiaiaiaatan Eo lo see Repeating scan unit E E Scan repeats or goes to the end scan condition here depending on the scan type Figure 31 Parameters needed for the ramp generation commands Name ramppt Set an E or I vertex point for the ramp Description As illustrated in figure 31 there are three E I vertex points needed to define a ramp waveform Vertex point 15000 14999 14998 15000 EPN 2000 1999 1998 2000 ramppt 7 i x Galvanostat pper 1 1000 gt 1000 for 1A range These vertex points take mV values in potentiostat mode and milli fractions of the full scale current Irange in galvanostat mode For example the command ramppt 0 500 sets the first ramp vertex to 500mV potentiostat mode or 500 thousandths of Trange galvanostat mode The command ramppt 0 500 will return the value loaded into index 0 SRS Stanford Research Systems 106 EC301 Potentiostat Galvanostat ZRA 7 Remote programming ramprt i x 7 3 Detailed command list Name ram
29. has been engaged from the front panel control loop is engaged big red CELL button is lit and the SET key is pressed to adjust TRACKING will light to indicate that cell polarization is moving with the knob This allows manually adjusting polarization while observing other cell characteristics thumb wheel scanning Most parameters can be locked in by re pushing the same key used to set them For example pushing SET once to adjust the E of a hold will allow will allow 4 to be freely changed with the knob Pushing SET again will lock the value in and disable the knob The value will also be locked in if a SET key from another section is pressed In general moving on to another setting will lock the previous one SRS Stanford Research Systems 29 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 1 Front panel 3 1 16 Configure Use this section to configure the remote interface LAN GPIB CONFIGURE and to cycle through the various display modes GPIB Torne DISPLAY EJ E Wa SRS stanford Research Systems 30 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 1 17 Remote status REMOTE STATUS O sro LOCAL O ACTIVITY REMOTE MODE ERROR O EXT TIMEBASE ASRS 3 1 Front panel The indicators in this section describe the status of the remote GPIB or LAN interface and the external timebase SRQ This indicator is on whenever a service request SRQ is gener at
30. panel auxiliary ADC input BNC Example SRE 2 Unmask the MESR status bits only MESE 8 Unmask the Aux 1 overload status bit from MESR Apply more than 10V to the rear panel Aux 1 BNC to cause a SRQ STB See that bit 6 SRQ of the status byte has been set Remove the overload on Aux 1 MESR Query the MESR register to clear the Aux 1 overload bit STB See that bit 6 SRQ has also been cleared in the status byte Name CLS clear all status registers CLS Description This command clears all the status registers INSR MESR and ESR It will also terminate all scans in progress Name errmsg Return the front panel s most recent error code or message Description This query only command returns errors that have been displayed on the front panel character display Since these errors disappear after a short time this command provides a way to always get the most recent error message The error codes returned with i 0 are unique to errmsg the front panel errmsg i errors They can not be decoded using errdcd See the errlst and errdcd commands on pages 98 and 98 for more information about error reporting Error report returned 0 Most recent error code Most recent error message Verbose form of most recent error message SRS stanford Research Systems 97 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name errlst Return the most recent system leve
31. programming 7 3 Detailed command list Name limitg Query if the CE Limit is active limitg eye bea eee i satin seats i Description limitg returns 1 if the CE limit is active 0 if the limit is inactive Use the celimt command to enable or disable the CE limiting SRS Stanford Research Systems 69 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 4 Cell switch Name ceenab Set or query the CE switch position Description Enable or disable the cell The red enable switch on the front panel will illuminate if the cell is enabled and the switch is pushed in ceenab i a Cell connection 0 Disabled Enabled Name cellon Query the cell connection Description This query only command returns the state of the cell connection As shown in figure 1 on page 18 this connection is made only if both the current interrupt cell switch and the front panel safety switch are closed Since the safety switch lights up only when both of these are closed this query tells you whether or not this light is on Cell connection cellon i Disconnected Either the current interrupt cell switch or the front panel safty switch is open safety switch red light is off Connected Both the current interrupt cell switch and the front panel safety switch are closed safety switch red light is on SRS stanford Research Systems 70 EC301 Potentiostat Galvanostat ZRA 7 Remote pr
32. range is the current range in use Measure ment accuracy will degrade from specifications during overloads CURRENT OVERLOAD SRS stanford Research Systems 23 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 1 Front panel 3 1 8 Mode Use the MODE key to cycle the EC301 through its various oper ating modes POTENTIOSTAT GALVANOSTAT POTENTIOSTAT control potential and measure current In this oe mode the EC301 controls the potential of the working relative to bau the reference electrode The counter electrode is driven to whatever potential is necessary within the 30 V or the user imposed com pliance limits to hold Vwr sense Vre at the control program voltage GALVANOSTAT control current and measure potential In this mode the EC301 controls cell current flowing through the working electrode The counter electrode is driven to whatever potential is necessary to hold this current at the programmed value ZRA Zero resistance ammeter hold two electrodes at the same potential In this mode the EC301 holds the counter and working electrodes at the same potential while current flows between them Current flow with no potential drop implies no resistance hence the name of the mode The relative potential is sensed with the WE SENSE and CE SENSE connections and the counter electrode is driven to hold this potential at Zero CALIBRATE This function is reserved for use by the fa
33. the cell to be held at a constant potential or current before the repetitive part of the waveform is applied Subsequent points are then output until the ppoint value is reached The waveform then loops back to output point P For example the command will tell the waveform generator to make room for the minimum number of two control points SRS stanford Research Systems 100 EC301 Potentiostat Galvanostat ZRA 7 Remote programming psteps x pdatap i x 7 3 Detailed command list Name psteps Set or query the pulsed waveform step size Description This is the current or potential increment applied to the pulsed waveform baseline 15000 14999 14998 15000 x 1 os Izango 2000 1999 1998 2000 1 1000 gt 1000 for 1A range This step size takes mV values in potentiostat mode and milli fractions of the full scale current Irange in galvanostat mode As illustrated in figure 30 the baseline is incremented after a control point is applied with its increment bit set pincrm x x 1 For example the command psteps 50 sets the step size to 50mV Name pdatap Set or query the pulse data waveform control point values Description Each of the possible six control points used to specify a pulsed waveform needs a voltage or current value 0125 Potentiostat mV 15000 14999 14998 15000 2000 1999 1998
34. the rest of the connections from the EC19 to the cell as normal Under these conditions the full 15 V potentiostatic polarization range is available 4 1 3 Grounded Counter Electrode Once you have removed the shorting bar from the rear panel of the instrument see Overview above you are ready to begin measurements in this configuration You may achieve somewhat improved noise performance by attaching a jumper between CE and signal ground When you tie the CE to Earth ground be aware that the full potentiostatic polarization range is not available In this configuration the potentiostatic set point dictates the potential between signal and floating ground The maximum polarization range under these conditions is 8 V 4SRS Stanford Research Systems 46 EC301 Potentiostat Galvanostat ZRA 4 Making cell connections 4 2 Working with grounded electrodes Figure 15 Grounding WE at the EC19 Reference Electrode a Figure 16 Grounded counter electrode configuration 4 2 Working with grounded electrodes Grounded electrodes are those inextricably connected to earth ground Figure 17 illustrates cathodic pro tection of a buried pipeline in which the counter and working electrodes are necessarily buried in and thus connected to earth Figure 18a illustrates the proper current circuit in this situation out of the power am plifier through the CE and WE electrodes through the WE shunt resistor and back to the power amplifier 4SR
35. these conditions are true e Galvanostat mode is in use e Positive feedback IR compensation is in use e Bias rejection is in use SRS stanford Research Systems 79 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 11 Reading single measurement results vlevel ilevel getaux i Name vlevel return an E measurement Description This query only command takes no arguments and returns a floating point number in volts For example if Vwe sense Vre happens to be 1 543V the sequence vlevel 1 543 will return that value Name ilevel return an J measurement Description This query only command takes no arguments and returns a floating point number in amps For example if Iwg happens to be 1 543mA the sequence ilevel 1 543e 3 will return that value Name getaux Get voltages from the rear panel auxiliary input BNCs Description This query only command returns voltage measurements made with the rear panel auxiliary input BNCs described on page 38 Voltage returned Auxiliary input 1 2 Auxiliary input 2 3 Auxiliary input 3 4 Comma delimited values from all three channels Example getaux 1 Query the voltage at auxiliary input BNC 1 1 723993 Volts SRS stanford Research Systems 80 EC301 Potentiostat Galvanostat ZRA 7 Remote programming avgexp i 7 3 Detailed command list Name avgexp Set or query the
36. triggers in general and section 3 2 6 on page 34 for a description of the rear panel scan trigger I Tp E Dap eg eee re l Rate 7 YE q Time Time a A linear current ramp program using SINGLE scan b A linear current ramp program followed by a simu type and J end condition lated jump to open circuit zero current using SINGLE scan type and OPEN CIRCUIT end condition The cell current and potential are uncontrolled when the return ramp finishes 5 Time c A linear current ramp program using CONTINUOUS scan type The triangle shaped program continues indefinitely Figure 24 Parameters used to set up a linear current ramp scan SRS Stanford Research Systems 58 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 2 Setting scan parameters galvanostat mode 5 2 3 Current step Figure 25 illustrates the parameters needed to specify a current step scan The procedure is as follows 1 Use the MODE key to select STEP 2 Cycle through the required parameters using SET and adjust values using the knob 3 Choose the scan end condition Figure 25 a illustrates the cell potential for the J end condition while 25 b shows it for OPEN CIRCUIT If the end condition is OPEN CIRCUIT the cell potential will be free to drift after the T wait time If the condition is J4 the potential will immediately return to J 4 Choose SINGLE or CONTINUOUS scanning Single scans illus
37. 1 Powerentry eccna 06 dw he eG ee ee Ble oa eee a aa de 3 2 2 GPIB interiac su sik ee eee a AAA EG ok a ORS 3 2 3 Ethernet interface i ss saoi e doada mate gud dea b d e 3 2 4 Current interrupt synchronization e ee 3 2 5 Timebase synchronization input e 3 2 6 Sean trigger input sa dosos e ee A ae ee Ge ee 3 2 7 Program E T Output sea 444 4 er Ro oe eee ee har eee Be a 3 2 8 Scan synchronization output s s s i eoi aa ee 3 2 9 Auxiliary ADC inputs 1 3 eee 3 2 10 Resistance temperature detector RTD input o o o 3 2 17 Grounding posts c e so iaae kB ASST da E AAA ee Oe amp SO o212 Raw analog Outputs e ss e scese era ea ek ee eh ae Bee G a S203 CR MOntOr 4 2 oe esd aan ed PERE ODS Mee eo Bee OS 3 2 14 Synchronous ADC input sies s ss adak ew ESS eee ee EEG 4 Making cell connections Floating operation e s 640 ew ke bb ee PAA CA ee ee ha ee a 4 1 1 cs en 5 IEEE 4 1 2 Grounded Working Electrode 2 0 000000 a AID oro Contents 4 1 3 Grounded Counter Electrode 2 2 46 4 2 Working with grounded electrodes 2 2 o 47 5 Performing scans using the front panel 50 5 1 Setting scan parameters potentiostat Mode o e 50 5 1 1 Cyclic voltammetry VJ as en a a a oe SE a 50 5 1 2 Linear sweep voltammetry LSV 1 0 0 00 0000 eee eee 52 5 1 3 DUEPS 4 edad dese a a se tee an ae eeedue kas 54 5 1 4 Holds 0 cala a 2 A ESS A a a E 56 5
38. 32 No remote amp CI limit ESB ESR sra FC 1 2 4 8 a 28 8 Figure 29 The status bit promotion diagram Enabling bits in the INSR MESR and ESR status registers allows them to set bits in the STB Enable these bits with the INSE MESE and ESE registers Properly configuring status bit promotion allows quick status byte STB queries to indicate problems SRS stanford Research Systems 99 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 16 Pulsed waveform generation commands pincrm 1 1 1 EN 4 a Increment baseline after hold Add value to baseline This is point 1 P T Ro T gt P P value 10 P value i O i A baseline 07 AA mes ROIS RS Re eee ee eee Gee i Seer eee ee eee eS eee ee ee ee eee a ee ee RAR Ty gt gt pincrm 0 0 0 Time les Do not increment baseline after hold Do not add value to baseline This is point 0 Figure 30 A very basic waveform illustrating the pulsed waveform construction parameters ppoint 7 i Name ppoint Set or query the number of pulse waveform points Description Pulsed waveforms may be specified with up to six control points with the number of points given by i 1 The waveform generator must be told how many points it will be using Allowed values 12 345 15 Figure 30 illustrates a waveform with only two control points The first point Po allows
39. 7 3 8 Analog output commands su iara de amaa nea a a k E a a aa 75 7 3 9 Voltage E measurement setup 2 2 ee 77 7 3 10 Current I measurement setup e 78 7 3 11 Reading single measurement results o ee 80 312 Streaming data s a ae be be ee RR wa ee eS eo ee ee ae a 82 7 3 13 Remote interface commands 0 0000 ee ee 86 1 3 14 Timebas commands sea aoa e 040 bea RR da RR E e 89 7 3 15 Status reporting commands e 90 7 3 16 Pulsed waveform generation commands 000000000 2s 100 7 3 17 Ramp generation commands i lt c eoe aaa 0 002 a e e ia ee 106 7 3 18 Arbitrary waveform generation commands e 111 7 3 19 Reading temperature measurements 2 0 a a 116 TA Programming examples a cs e oc aa b eaa hk e sa E AAA 117 7 4 1 Normal pulse ae soros a 6450 444 0 emb a ae 117 7 4 2 Cycle voltammetry usara A A e Be ak a 118 7 4 3 Current interrupt IR compensation e 119 7 4 4 Arbitrary wavelotm te ob m e A ee a a ad ee a 120 Bibliography 121 A Measuring cell voltages at the cell 122 Contents B Pinouts B l Gell interface 25 pins 40 amecae RR EE Ee eG eG Re eS B2 RED unterface 6 pits pe ee eho ek ee Deed ee Oop Wee eee 28S C Major symbols and abbreviations Alphabetical command index 124 124 124 1 General information 1 General information 1 1 Safety and preparation for use Warning Dangerous voltages
40. Argument formats Table 3 summarizes the number formats expected for each argument designator Argument designators Good examples 1900 0 1 5 78 5 200 one 1 34 0 0 8 14189 Table 3 Number formats expected for each argument designator Numbers written in scientific notation will not be recognized as allowed arguments SRS stanford Research Systems 64 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 Detailed command list 7 3 1 Firmware and hardware revisions Name fpgarv Query the FPGA revision number fpgarv Description The instrument s FPGA revision number is important for firmware upgrades 7 3 2 Program E I setup with external input Name setvol Set or query DC bias voltage Description This command provides an easy way to control a DC voltage with out setting up a scan mV 15000 14999 14998 15000 For example the sequence setvol i ecmode 0 ceenab 1 setvol 1000 setvol 1000 will set up a program voltage of 1V in potentiostat mode The setvol query command will return a value in the same format as the setting This command is not allowed in galvanostat mode zra mode or if the unit is in direct control mode SRS stanford Research Systems 65 EC301 Potentiostat Galvanostat ZRA 7 Remote programming setcur x addscn i 7 3 Detailed command list Name setcur Set or query DC bias for the cur
41. BNC output Enc is opposite that reported on the front panel displays The voltage is thus Egnc Vre Vwe sense We invert the polarity here to correct the sign of the cell impedance Zeen calculated with Eno Leal gt Irange x Igne where frange is the current range in use and gnc is the voltage at the CURRENT BNC output See figure 2 for an illustration of BNC versus display polarities BIAS REJECTION Bias rejection attempts to subtract off the DC component of the analog output voltages This can be useful when making AC response measurements in the presence of a DC hold Removing the DC component of a signal can allow the use of more sensitive input ranges on external equipment like frequency response analyzers When BIAS REJECTION is pushed the EC301 will immediately average Vre Vwe sense and Iwg over a ls window It will then subtract those average values from all subsequent front panel Egnc and Igne outputs The averages will not update until bias rejection is turned off and then back on Note that the RAW E and RAW I outputs on the rear panel always provide the Vre Vwe sense and Iwg measurements with no filtering or bias rejection Bias rejection affects both analog outputs simultaneously when engaged from the front panel gt but can be limited to either output when set up using the remote interface The individual rejection levels can also be set arbitrarily instead of being automatically detected
42. EC301 Manual October 2 2014 Contents 1 General information Safety and preparation for use Symbols you may find on SRS products da die sarp EEEL Specifications Serial number and firmware revision 1 1 1 2 1 3 1 4 2 EC301 basics Software Functional block diagram Polarity convention Connecting the EC19 to the EC301 2 1 2 2 2 3 2 4 3 Operation 3 1 3 2 4 1 2 4 1 2 4 2 Necessary Items EPS fice dont Bee ES Front pan l vea Pee eee bd A EOE AY Ee ete he ae 3 1 1 POWeErOn reset he Be LARA ERE Mae ERR CRRA ER ERS EE 3 1 2 Bandwidth limit ea RS ee a ed 3 1 3 A E Bete a pe Ge ee ee a aoa eee ee eee a eae 3 1 4 A 3 1 5 External electrometer swis d ee pel Se es e A 3 1 6 Voltage cia so ey Fw e A a e 3 1 7 A s a a po D E aaa n ae Ea aa ak a E es BS eae amp 3 1 8 Mode es sda eame ee EHR Ee Re Re a e a e a ee ee eS 3 1 9 Rotating electrode s soos a eaa 2444 AA a wad S140 Analog Output ee v0 6 oe o eee Bea E a de A S110 Current ranges criar AAA a a 3 1 12 IR COMPERSALIO fac fe e dote o es aed ds pe rd rd ees a ed 31 13 External input oso se m easan aoka a aa eai e aa aa a Re 3 1 14 Measurement setup control 2 2 a S15 Kib fe ee 4k Wee BE o A da a Ol lor oi A ee ee eo Oe ee EN SL Remoterstatus s sers 06 406d bbe kd bebe ean doe w eee degen bee od Rear patel oceane eee os Sade ad ag Seek A EMER EAD ES lid eS 3 2
43. N TRIGGER inputs Start waveform playback automatically This will engage the control 1 g Stop waveform playback and open the control loop This will also loop in whichever mode range combination specified with arbtyp arbrun i mode range combination specified with arbtype but playback will not begin until a falling edge is received at the rear panel SCAN TRIGGER input Arm waveform playback This will engage the control loop in whichever 2 Only one scan type ramp pulse hold or arbitrary can be armed at any one time The most recent scan type to be armed will be run when a trigger is received at SCAN TRIGGER SRS stanford Research Systems 115 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 19 Reading temperature measurements Name getrtd get temperature reading Description This query only command returns the RTD probe measurement in C gotrtd Example getrtd 52 75 Degrees Celsius Name rtdohm get the RTD probe resistance Description This query only command returns the RTD probe resistance in ohms rtdohm Example rtdohm 50 35 Ohms SRS Stanford Research Systems 116 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 4 Programming examples 7 4 Programming examples 7 4 1 Normal pulse As described by Bard and Faulkner 1 the normal pulse voltammetry waveform involves a base potential and a series of increasing steps The follow
44. ND a Two terminal cell b Three terminal cell SIGNAL GROUND SIGNAL GROUND c Four terminal cell d ZRA mode Figure 12 Making cell connections SRS stanford Research Systems 44 EC301 Potentiostat Galvanostat ZRA 4 Making cell connections 4 1 Floating operation Probing electrode voltages with a standard oscilloscope probe can cause problems with grounding and noise See appendix A for more details 4 1 Floating operation The EC301 was designed with floating operation in mind Users may operate on a Working Electrode WE that is intrinsically grounded or they may wish to strap the Counter Electrode CE to earth ground for safety reasons The EC301 will accommodate those measurements but there are some configuration adjustments that must be made 4 1 1 Overview For floating operation remove the factory installed shorting bar that ties the signal ground and the floating ground together see Fig 13 Pull the bar away from the instrument to remove it Figure 13 EC301 grounding bar installed The signal ground is an internal reference which is maintained at close to chassis ground potential The floating ground is a separate reference that is free to reach a potential difference up to 8 volts from signal ground In the event the potential between signal and floating grounds exceeds this limit the instrument 4SRS Stanford Research Systems 45 EC301 Potentiostat G
45. Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 9 Voltage E measurement setup Name eadcrg Set or query the full scale range of the internal E measure ment Description The instrument defaults to a 15V measurement range This can be reduced to increase measurement resolution eadcrg i 0 Name eadcf1 Set or query the low pass filter in front of the E ADC Description No description eadcf1 i No filter 10Hz lowpass 10kHz lowpass anti alias SRS stanford Research Systems 77 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 10 Current J measurement setup Name irange Set or query the current range Description No description 1 Current range _i Current range irange i You cannot do irange if you are autoranging Name iadcf1 Set or query the low pass filter in front of the J ADC Description No description iadc 1 i 0 10Hz lowpass 10kHz lowpass anti alias SRS stanford Research Systems 78 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name irnaut Set or query the I autoranging mode Description The current measurement circuit can automatically change ranges when the measured current is at the extreme end of a range Autoranging irnaut i Autoranging of the I V converter is disallowed if any of
46. S Stanford Research Systems 47 EC301 Potentiostat Galvanostat ZRA 4 Making cell connections 4 2 Working with grounded electrodes through floating ground If however the floating and signal ground binding posts described in section 3 2 11 are left connected current can bypass the WE entirely Figure 18b shows current flowing out of the CE and being returned to the power amplifier through earth ground which has a low resistance connection to signal ground The rear panel signal and floating grounds should thus be disconnected when making measurements with grounded electrodes The rear panel ground banana jacks should only be disconnected when necessary Reconnect them when using isolated cells to improve frequency response D O CD Q ws WF y G CE CE RE WE SENSE SENSE WE GROUND N J Soil surface Anode y Cathode buried pipe Figure 17 Buried and inextricably grounded electrodes used in cathodic protection SRS stanford Research Systems 48 EC301 Potentiostat Galvanostat ZRA 4 Making cell connections 4 2 Working with grounded electrodes Floating ground DN Soil surface CE Current flow Earth WE S ground 777 shunt resistor a Proper current flow with floating and signal ground posts disconnected Nx Signal ground o connected to earth ground Floating Soil surface ground paa Earth 9 ST
47. alvanostat ZRA 4 Making cell connections 4 1 Floating operation will not be damaged In this case the CE limit will be activated and the potential across the cell will not be well controlled The EC301 grounding scheme leaves all the connectors on the chassis unaffected by floating operation Instruments such as oscilloscopes and frequency response analyzers often tie other instruments chassis to earth ground once a BNC cable is attached between them This is permissible even when the EC301 is floating because the BNC shells are tied to chassis ground and not floating ground This enables EIS electrochemical impedance spectroscopy even on working electrodes that must float Floating operation necessitates some trade offs in performance The EC301 specifications only apply when the signal and floating grounds are connected on the rear panel by the supplied shorting bar i e when the instrument is not floating 4 1 2 Grounded Working Electrode Reference Electrode _ Figure 14 Grounded working electrode configuration Once you have removed the shorting bar from the rear panel of the instrument see Overview above install it between the two banana jacks on the EC19 labeled WE and SIGNAL GROUND see Fig 15 The shorting bar provides a low impedance path between the intrinsic ground at the cell and the EC301 internal reference ground improving noise performance and adding stability to the current meter Make
48. arch S ystems 12 1 3 Specifications EC301 Potentiostat Galvanostat ZRA 1 General information Front panel connectors e External input 15V analog input in p Input impedance 10kQ e Rotating electrode output B 0 gt 10V analog output otentiostat mode 2V in 50pF NC Accuracy 1 of setting 5mV Output impedance 100 10mA max output current e Voltage E output BNC 15V analog output Accuracy 0 2 of Vre VWE sense 5mV Output impedance 500 10mA max output current e Current I output BNC 2V analog input Accuracy Iwg within 4 0 5 of Venc x Lange 3 Accuracy Iwg within 4 1 3 Specifications galvanostat mode E 0 2 x Tange 1 A range 0 2 of Venc x Tange Output impedance 500 10mA max output current S RS Stanford Research S ystems 13 E 0 2 x Irange other ranges EC301 Potentiostat Galvanostat ZRA 1 General information Rear panel connectors e Timebase input BNC Frequency 10MHz Level 1Vpp nominal e TTL measurement synchronization BNCs 1 3 Specifications Current interrupt and scan synchronization outputs scan trigger input Program E I output BNC 15V analog output Accuracy 0 2 of total program voltage internal sources external input 5mV Output impedance 100 10mA max output current Auxiliary ADC input BNCs Three 10V analog to digital inputs input impedance 100kQ 1mV resoluti
49. bitrary waveform Description This query only command returns the number of points that have been set via the arbset command It may be used to verify that all arbset arbpts commands were processed properly Returned parameter Values 012159 Name arbdly Set or query the hold time for the first arbitrary waveform point Description The EC301 can hold the first point in an arbitrary waveform to let a cell settle This command sets the extra time that the point should be held Ais arbdiyt i relative to the following points 01 2 10 Name arbdiv Set or query the playback rate divider for the arbitrary waveform generator Description The default playback rate for arbitrary waveform points is 1 megasample per second This command allows reducing that rate by a factor of i ee 12 3 1024 For example the sequence arbdiv 1000 arbdiv 1000 will set the playback rate to gt 1ksps or 1000 points per second Name arbend Set or query the end condition for arbitrary waveform scans Description Arbitrary waveform scans can end by either maintaining control at the first point of the waveform or by releasing control open circuit arbend i 0 Control is maintained at the first waveform point default Control is released open circuit SRS stanford Research Systems 112 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name arbcyc S
50. bitrary waveform generation commands EN 4 Repeating scan unit D e D Scan ends with control at the Po i Doo Dy first D y point tus X arbdiv lt gt arbdly seconds D D gt Time Figure 32 Illustration of an arbitrary waveform with five arbset points and three repetition cycles The time between ARBSET points is always lus x arbdiv Repeat points to get longer hold times Name arbrst Reset the arbitrary waveform generator Description The arbitrary waveform generator should be reset before a new waveform is programmed This reset disables the generator and sets the default conditions listed in table 10 Sot with Default value A waveform type must be f y Waveform arbtyp Undefined chosen with arbtyp before type points can be entered with arbset poms em o arbpts points brst Z SREE Clock arbdiv 1 divider CN E arbcyc 1 cycles By default the instrument will End e arbend E h loop back to hold the first point condition in the waveform when the scan ends By default triggering via the Scan trigger arbrun Internal SCAN TRIGGER input is disabled Table 10 Arbitrary waveform generator parameters after issuing the arbrst com mand SRS Stanford Research Systems 111 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name arbpts Query the number of points in the ar
51. capable of causing injury or death are present in this instrument Use extreme caution whenever the instrument covers are removed Do not remove the covers while the unit is plugged into a live outlet Line fuse Verify that the correct line fuse s are installed before connecting the line cord Fuse size is 3AB 3AG slo blo 6 3 x 32mm For 100V 120V use a single 3 A fuse for 220 V 240 V use two 1 5 A fuses Line cord The EC301 has a detachable three wire power cord for connection to the power source and to a protective ground The exposed metal parts of the instrument are connected to the outlet ground to protect against electrical shock Always use an outlet which has a properly connected protective ground Service Do not attempt to service or adjust this instrument unless another person capable of providing first aid or resuscitation is present Do not install substitute parts or perform any unauthorized modification to this instrument Contact the factory for instructions on how to return the instrument for authorized service and adjustment SRS stanford Research Systems 5 EC301 Potentiostat Galvanostat ZRA 1 General information 1 2 Symbols you may find on SRS products 1 2 Symbols you may find on SRS products Alternating current Caution risk of electric shock Frame or chassis terminal Caution refer to accompanying documents Earth ground terminal SRS stanford Research Systems 6 EC301 Potentiostat Galvan
52. ce spectroscopy Using the setup shown in figure 27 the SR780 supplies the stimulus for swept sine or FFT based mea surements via the external input BNC It then can calculate the complex cell frequency response as FFT2 Res 1 esponse Fay 1 for FFT based measurements or as spectrum2 Response 2 spectruml using the swept sine mode The cell impedance Zeen can be calculated from this using spectrum2 Leel 3 Its x spectruml where J is the current range 10mA 1004A etc SRS stanford Research Systems 63 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 Remote programming The EC301 may be remotely programmed via either the GPIB or ethernet interfaces When using the ethernet interface be advised that some personal firewall systems will terminate idle connections 7 1 Command syntax Communication with the EC301 is done with ASCII characters Commands may be in either UPPER or lower case and may contain any number of embedded space characters For example the commands ECMODE 1 ECMODE ecmode 1 will all put the instrument in galvanostat mode Multiple commands may be sent on one command line by separating them with semicolons The individually sent commands ecmode 1 clbwth 4 irange 1 can be sent simultaneously with ecmode 1 clbwth 4 irange 1 following which the EC301 will buffer and then execute the command string from left to right 7 2
53. cted to should exceed 10kQ to keep loading errors below 1 SRS stanford Research Systems 41 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 13 CE monitor CE 3 OUTPUT 3 2 Rear panel This output provides the counter electrode CE voltage relative to floating ground divided by 3 If signal and floating grounds are connected together this output will span 10 V as the CE spans 30 V As with the raw E and J outputs this signal is not affected by bias rejection or filter settings The output resistance of this source is 500 The input resistance of whatever this is connected to should exceed 10kQ to keep loading errors below 1 S RS Stanford Research Systems 42 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel 3 2 14 Synchronous ADC input This 10 V analog input allows sampling external signals simulta SYNC ADC neously with the E and J measurements The EC301 has separate ADCs devoted to the E I and synchronous ADC measurements All three ADCs share the same sample control signal to ensure simultaneous measurements INPUT SRS stanford Research Systems 43 EC301 Potentiostat Galvanostat ZRA 4 Making cell connections 4 Making cell connections Figures 12a b and c illustrate how the EC301 should be used with cell configurations in potentiostat and galvanostat modes Figure 12d illustrates typical cell connections during an experiment using ZRA mode SIGNAL SIGNAL GROUND GROU
54. ctory 3 1 9 Rotating electrode This DC voltage output can be used with an external control unit ROTATING ELECTRODE to control the speed of rotating working electrodes Use the SET key to adjust the output voltage within 0 gt 10V This output can source a maximum of 10 mA The input impedance of the external control unit must be larger than 1 kQ to achieve the maximum 10 V output SRS stanford Research Systems 24 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 1 Front panel 3 1 10 Analog output This section contains the VOLTAGE and CURRENT analog outputs ANALOG OUTPUT as well as the BIAS REJECTION and 10 Hz LOWPASS FILTER s controls for modifying the outputs VOLTAGE output Epnc This output is the potential of the ref erence electrode with respect to the working electrode optionally o subjected to a 10 Hz lowpass filter and or bias rejection The 15 LOW PASS V output range is the same as the maximum polarization range VOLTAGE CURRENT CURRENT output Ignc This output is proportional to current flowing in the working electrode Iwg optionally subjected to a 10 Hz lowpass filter and or bias rejection The output voltage is 50 2 OUTPUTS i LOAD WITH210kQ given by Iwe Ipnc 1V x range where Jrange is the current range in use 1 mA 10 mA etc As described in section 2 3 Ignc becomes more positive when current flows into the working electrode cathodic current The polarity at the VOLTAGE
55. d program continues indefinitely Figure 21 Parameters used to set up a step scan SRS Stanford Research Systems 55 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 1 Setting scan parameters potentiostat mode 5 1 4 Holds Figure 22 illustrates the parameters needed to specify holds or timed holds These scans must end in the OPEN CIRCUIT condition and the scan type can only be SINGLE Only MANUAL trigger mode is allowed The remaining setup procedure is as follows 1 Use the MODE key to select HOLD or TIMED HOLD 2 Set the Ej and T parameters using SET and the knob 3 Choose the trigger mode MANUAL allows the GO ARM key or the remote interface to start the hold See section 5 4 on page 61 for a better description of scan triggers EXTERNAL mode is not allowed Es Open circuit Indefinite E 4 Time Scan ended manually gt a A indefinite hold program Holds must end in the OPEN CIRCUIT condition Es Open circuit T o j E ot Time b A timed hold program Control is automatically released after the T hold time Figure 22 Parameters used to set up a regular and timed hold SRS stanford Research Systems 56 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 2 Setting scan parameters galvanostat mode 5 2 Setting scan parameters
56. d on the preceding page via the MESE register this one set the MESW bit in the status byte The MESE query returns the value of the Measurement Status Enable Register The MESE i command queries only bit i MESE 7 i j When the instrument sets a bit in the Measurement Status Register and the corresponding bit is set in the Measurement Status Enable register by the user bit 1 MESW of the Status Byte is set This causes a SRQ if bit 1 in the Status Byte Enable register is set Example MESE Returns the register value in decimal format MESE 2 Returns 0 if bit 2 is cleared or 1 if it is set MESE 48 Sets the register value to 48 bits 4 and 5 set MESE 7 0 Clears bit 7 SRS stanford Research Systems 95 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name STB Query Status Byte values Description This command returns values from the Status Byte register Send ing STB will return the entire register value in decimal format while sending STB i will only return bit i Reading this register will not clear it it must be cleared by reading the registers that feed it See figure 29 on page 99 for a description of how status bit values are promoted to this register Table 9 lists the conditions corresponding to the register bits INSY An unmasked bit in the Instrument Status Register described on page 92 has been set 1 MESW An unmasked bit in the Measurement Status Register d
57. dcntr1 i progrm 7 3 Detailed command list Name dentr1 Set or query the external input s direct control mode Description This command enables or disables the external input while engaging and disengaging cell control Setting 0 Voltage at external input ignored Voltage at external input applied to cell This is useful when you have an external source for your entire stimulus and you don t want to use the internal sources Sending dcntrl 1 works like pushing DIRECT CONTROL on the front panel the control loop will close with the control voltage taken from the external input BNC However sending dcntrl 0 will only open the control loop if the external input has been put in charge with dcntrl 1 not if an internally generated scan or hold is running This command will generate an error if an internally generated scan or hold is already running Make sure all control has been released before sending dcntr1 1 Name progrm Read the program E I voltage Description This command queries the total voltage program input to the con trol loop 15 000 gt 15 000 The program input is the sum of voltages from the external input BNC and from internal sources This command is useful during current interrupt IR compensa tion as the values returned should represent the cell voltage with any IR drop removed Returned values are formatted as floating point volts For example the sequence ecmode O setvo
58. e EC301 can accept standard 1002 Pt RTD probes for logging RTD INPUT experimental temperatures The probe temperature is determined weg with a 4 wire measurement of the probe resistance As illustrated in figure 10 commercial 4 wire RTDs normally have two wires of 2 o gg the same color connected to one end of the resistive sensor and 56 lt lt two wires of a different color connected to the opposite end One m m Z i of each pair carries the drive current used in the measurement and the other is used to sense the voltage induced by this current The drive and sense leads are interchangeable WW 1002 Pt RTD Figure 10 Commercial 4 wire RTD probes have two wires with the same color attached to each end These 4 wire sensors are connected to the EC301 in one of two electrically identical ways illustrated in figure 11 Notice that the signs of the DRIVE and SENSE inputs match for the same color of wire Any other wire configuration will give no temperature reading when the probe is connected UR Eog SiS ANQUI ppa HEZIZ Guess Guess 22 c mm COCA i gti i O Mo Figure 11 4 wire probes can be connected to the EC301 in one of these two ways RTD sensor wires are connected to the RTD input using 5 pin Weidmuller plugs Weidmuller part number 169045 These plugs use a tension clamp to hold the wires in place To install the wires 1 Hold the plug in front of you with the five small holes on top and the fi
59. ed All buttons except LOCAL will be disabled after sending lockfp 1 Pressing LOCAL will unlock the front panel and reset lockfp to 0 Name ifcclr Reset the remote interface Description This command clears the remote interface s transmit and receive queues If the instrument s reply to a query isn t read before another query is issued an error occurrs and new reads are forbidden Sending ifcclr when this happens will clear this condition allowing new queries to be sent and their replys ifcclr to be read The REF bit in the instrument status register described on page 92 is set when multiple queries are sent without a read Sending ifcclr will not clear this bit it should be cleared with a normal INSR query Name macadr return the EC301 s Media Access Control MAC address macadr Description This query only command takes no arguments and returns the MAC address SRS stanford Research Systems 87 EC301 Potentiostat Galvanostat ZRA 7 Remote programming vidmsg i string nulcmd i 7 3 Detailed command list Name v dmsg Display a string on the character display Description This set only command prints the input string argument to either the first or second line of the front panel vacuum fluorescent character display The string must be less than 24 characters long and may not contain any spaces tabs or other whitespace characters Display line Fol Top line For example the command
60. ed by the EC301 It will stay on until the status register INSR MESR or ESR causing the SRQ is cleared See figure 29 on page 99 for a description of how status bit values are promoted to cause SRQs ACTIVITY This indicator flashes when there is activity on the re mote interface REMOTE MODE This indicator is on when the front panel is locked out by the remote interface No front panel adjustments may be made until the LOCAL key is pressed ERROR This indicator flashes when there is a remote interface error such as an illegal command or an out of range parameter EXT TIMEBASE The EC301 can accept an external 10 MHz timing signal to improve the accuracy and stability of automatic scans This indicator will light when such a timing signal is detected LOCAL The remote command LOCKFP can lock out the front panel keyboard Use the LOCAL key to exit this mode and enable the front panel keys S RS Stanford Research Systems 31 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel 3 2 Rear panel IEEE 488 ETHERNET a SCAN SCAN PROGRAM 10MHz TIMEBASE REME INTERFACE sY ic TRIGGER SYNC E I Apc ADC2 ADC3 g ion e For laborator OUTPUT INPUT OUTPUT OUTPUT INPUT INPUT INPUT AC POWER CHASSIS GROUND SIGNAL GROUND 3 SYNC ADC 90 VAC to 260 VAC FLOATING ISRS STANFORD RESEARCH SYSTEMS MADE IN U S A ota UNO OUTPUT INPUT 3 2 1 Power entry The power entry module is used to fuse the
61. end in the OPEN CIRCUIT zero current condition and the scan type can only be SINGLE Only MANUAL trigger mode is allowed The remaining setup procedure is as follows 1 Use the MODE key to select HOLD or TIMED HOLD 2 Set the J and T parameters using SET and the knob 3 Choose the trigger mode MANUAL allows the GO ARM key or the remote interface to start the hold See section 5 4 on page 61 for a better description of scan triggers EXTERNAL mode is not allowed Indefinite Time 0 gt Scan ended manually Time a A indefinite current hold program Holds must b A timed current hold program Control is automat end in the OPEN CIRCUIT zero current condition ically released after the T hold time Figure 26 Parameters used to set up a regular and timed current hold SRS stanford Research Systems 60 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 3 Basic scan controls 5 3 Basic scan controls Once a scan is configured the GO ARM PAUSE ADVANCE and STOP keys control how it will execute PAUSE Q Pressing the GO ARM key is one way to send a scan trigger il described in section 5 4 This will begin a scan in MANUAL trigger mode or arm the instrument in EXTERNAL mode The PAUSE key freezes the scan wherever it happens to be Pressing it again will resume the scan The ADVANCE key increments the scan stage For example pressing this during the
62. entiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name INSR Query the Instrument Status Register Description This command returns values from the Instrument Status Register Sending INSR will return the entire register value in decimal format while sending INSR i will only return bit i Reading the register will also clear it Sending ISNR will clear the entire register while sending INSR i will only clear bit i Table 7 lists the conditions corresponding to the register bits See figure 29 on page 99 to see an overview of all status registers INN A PS mca Selftest Failure the selftest has failed Keypress Event a key was pressed on the front panel in local mode Knob Rotation a parameter was changed by rotating the knob in local mode Remote Set a remote set command not a query was issued INSR i 4 CRC Current Range Change there was a change in the current I range a E 19 ETA External Timebase Acquired achieved lock to 10MHz timebase External Timebase Lost lost lock to 10MHz timebase An error has been posted that can be queried with errlst 15 REF Query Refused a previous query has not been completely read Perform read or send ifcclr Table 7 The Instrument Status register bits Example INSR Returns the Instrument Status register value 0 gt 65535 INSR 4 Returns 0 if bit 4 CRC is cleared or 1 if it is set SRS stanford Research
63. ernal clock The external source should be greater than 1V peak to peak and should be within 2 ppm of 10 MHz 10MHz TIMEBASE INPUT SRS stanford Research Systems 33 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel 3 2 6 Scan trigger input This input allows starting an automatic scan with external equip ment As illustrated in figure 8 an falling edge here will begin the SCAN AS TRIGGER scan within Lys The EC301 must be armed from the front panel or the remote O interface to use this input See section 3 1 14 on page 29 to set this condition from the front panel See the trgarm command described INPUT on page 73 to arm with the remote interface Falling edge Additional edges ignored starts scan until the EC301 is rearmed Scan trigger Program E I Scan sync Scan begins with T delay a Single scan Falling edge Additional edges ignored starts scan until the EC301 is rearmed Scan trigger Program E I Scan sync Falling edge output every time scan is repeated Scan begins with T delay b Continuous scan Figure 8 Timing diagrams for the SCAN TRIGGER input and the SCAN SYNC output using falling edge trigger polarity SRS stanford Research Systems 34 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel Why do these scans
64. escribed on page 94 has been set e EE ot use Pr a may There is a message available in the GPIB queue 5 ESB An unmasked bit in the Standard Event Status Register described on page 90 has been set SRQ Service request See the SRE command described on the next page for more information Set when the remote interface s receive queue is full Table 9 The Status Byte Register bits SRS stanford Research Systems 96 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name SRE set or query bits in the Status Byte Enable register Description The SRE i command sets the Status Byte Enable register to the decimal value i 0 255 The SRE i j command sets bit i 0 gt 7 to j 0 or 1 As shown in figure 29 on page 99 bits enabled in the STB register via the SRE register set the SRQ bit The SRE query returns the value 0 255 of the Standard Event Enable Register The SRE i command queries the value 0 or 1 of bit i 0 gt 7 When the instrument sets a bit in the Status Byte register and the corresponding bit is set in the Status Byte Enable register by the user bit 6 SRQ of the Status Byte is set The front panel SRQ light described in section 3 1 17 on page 31 will SRE 7 i j also light up This can be used as a general purpose indicator for a condition described by the status bits The example below describes using SRQ to indicate an overload at the rear
65. et or query the number of repetitions for arbitrary wave form scans Description Arbitrary waveform scans can be set to repeat either a finite or infinite number of times arbcyc i Repeat an infinite number of times The user can end the infinite loop by sending arbrun 0 Repeat i number of times The scan will end in the 1 2 3 4 1024 condition set by arbend Name arbset Set an arbitrary waveform datum Description This command programs arbitrary waveform data on a point by point basis Each point is specified by an index i and a datum j Waveform points are played beginning with i 0 and up to 16 000 points can define the waveform The datum type is set by arbtyp Potentiostatic datum types have units of mV while galvanostatic types have milli range units For example if the datum type is 5 corresponding to galvanostat mode in the 1mA range the datum will have units of yA E Potentiostat 15000 14999 14998 15000 arbset i j Galvanostat 1000 999 998 1000 1A range Galvanostat 2 sats all others 2000 1999 1998 2000 Each arbset produces an error code reply from the EC301 If the reply to arbset is non zero it signifies an error Every arbset must be followed by reading the error code reply from the EC301 SRS stanford Research Systems 113 EC301 Potentiostat Galvanostat ZRA 7 Remote programming arbget i
66. f the end condition is OPEN CIRCUIT the cell potential will be free to drift after the T wait time If the condition is 41 the potential will immediately return to E Choose SINGLE or CONTINUOUS scanning Single scans illustrated in figures 21 a and b go to the end scan condition after the Tz wait time Continuous scans illustrated in figure 21 c step back to E after the T2 wait time and repeat the entire step program indefinitely Choose the trigger mode MANUAL allows the GO ARM key to trigger the scan while EXTERNAL mode requires the rear panel scan trigger input See section 5 4 on page 61 for a better description of scan triggers in general and section 3 2 6 on page 34 for a description of the rear panel scan trigger SRS stanford Research Systems 54 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 1 Setting scan parameters potentiostat mode e a Time E gt Open circuit e ES penny oT Tai me ME Ap AE lt T am Ty Time a A step program and typical I vs E plot b A step program followed by a simulated jump to using SINGLE scan type and Ej end condi open circuit using SINGLE scan type and OPEN CIRCUIT tion end condition The cell potential is uncontrolled when the T wait time finishes E Ep ooo y Ty To T To Bsc T l T Time c A step program using CONTINUOUS scan type The rectangle shape
67. finished waveform The points all except Po can also instruct the baseline to increment when their hold times have expired 123 45 i 0 Do not add this point s value to the baseline Add this point s value to the baseline 0 Increment baseline after the point s hold has expired Leave baseline unchanged after this point The i parameter chooses the control point to set or query The j parameter selects whether or not the selected control point s value set with pdatap will add to the baseline in the final waveform The k parameter selects whether or not the baseline should be incremented after the point s hold has ended For example the P point shown in figure 30 is configured with the command pincrm 1 1 1 to have its value added to the baseline and for the baseline to increment after the T hold has expired The first Po point in a pulsed waveform definition is unique It allows a non repeating hold to be applied to the cell before a pulsed waveform train is applied pincrm bits set for this point will be ignored and queries will always return 0 0 0 SRS stanford Research Systems 103 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name plimit Set or query the number of steps in a pulsed waveform Description This command sets the number of steps the baseline will make in a pulsed waveform Parameter Range x 1 2 3 1048575 220 1 plimit
68. float SRS stanford Research Systems 122 EC301 Potentiostat Galvanostat ZRA References 5 STANFORD RESEARCH SYSTEMS MODEL SR560 LOW NOISE PREAMPLIFIER FILTER CUTOFFS Hz GAIN MODE RESET J w PAPI a on Ei En marasa Loss m Doa col pd 2 ea y RE ag PE 2 ar WE sense WE sense 4 lt d a Correct Measurement buffered by high impedance dif b Correct Measurement made directly with a handheld ferential amplifier the SR560 is shown meter To oscilloscope WE WE sense lt c Incorrect Connecting the ground pigtail of an oscilloscope probe to WE Figure 37 Correct and incorrect ways to make cell voltage measurements with external instruments SRS Stanford Research Systems 123 EC301 Potentiostat Galvanostat ZRA References B Pinouts B 1 Cell interface 25 pins Pin Main voltmeter RE WE SENSE output ZRA voltmeter CE SENSE WE SENSE output Table 11 Pinout for the front panel cell umbilical DB25 connector EN ES Ea EA E EA EN EA EJ B 2 RTD interface 5 pins SRS Stanford Research Systems 124 EC301 Potentiostat Galvanostat ZRA References Pin High side voltage sense SENSE Low side voltage sense SENSE Signal ground GROUND Current source DRIVE Current sink DRIVE Table 12 Pinout for the rear panel RTD connector numbered left to right SRS stanford Research Systems 125 EC301 Pote
69. forward ramp of a CV scan will start the return ramp Pressing this during the return ramp will skip to the GO ARM ADVANCE gt gt STOP Ble ie end scan condition The STOP key terminates the scan and releases cell control This does not simply take the scan to the scan end condition control is always released Use the ADVANCE key instead to skip to the end of a scan 5 4 Triggering scans A configured scan will start once the EC301 receives a scan trigger This can come from the front panel GO ARM button the rear panel scan trigger input or the remote interface 5 4 1 Triggering a scan from the front panel As described in section 3 1 14 on page 29 the front panel GO ARM key will start a scan if the trigger mode is set to MANUAL Pressing this in the EXTERNAL trigger mode will arm the instrument control will engage but scanning will wait for the scan trigger input The GO ARM key will try to engage cell control to begin a scan in both trigger modes lighting the ENABLE switch Make sure to allow this by pressing this switch to the on position 5 4 2 Triggering a scan with the scan trigger input As described in section 3 2 6 on page 34 the rear panel scan trigger input allows fine control over when the scan begins This can help to synchronize external data acquisition during fast scans 5 4 3 Triggering a scan from the remote interface The scan trigger remote commands are described i
70. have flat tops Figure 8 illustrates both CV and LSV scans triggered by the rear panel scan trigger input Since the OPEN CIRCUIT end condition isn t allowed for this trigger mode LSV scans must track back to their initial state after T making them look like CV scans with flat tops The two scans would look identical for Ta 0 SRS stanford Research Systems 35 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel 3 2 7 Program E I output This output is a copy of the input to the EC301 s control circuitry PROGRAM As illustrated in figure 1 it is the sum of the external input and E I the internal scan voltages When used with current interrupt IR compensation this output provides the corrected potential applied to the working electrode It can be used to plot IR compensated data on xy plotters and OUTPUT displays This output will reflect the input to the EC301 s control circuitry even when the control loop is open For example starting a 1V hold from the front panel without any external input voltage will move PROGRAM E I to 1V Stopping the hold won t change this output it will remain at 1V until a new scan is configured and run Note that the polarity for this output is consistent with the front panel VOLTAGE output described in section 2 3 on page 19 SRS stanford Research Systems 36 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel 3 2 8 Scan synchronization output
71. he external input A will be applied to the cell according to the American Polarity Con 2 V GALVANOSTAT vention described in section 2 3 This input has unity gain 1 V applied at the input will change Vwe SENSE VRE by 1 V The input thus accepts the full 15 V allowed polarization range In galvanostat mode controlled current is given by Vext Vprog 1V where Voxt is the voltage applied at the external input and Vprog is the internally generated program voltage Currents greater than 2 x range or 1 A will generate overloads so the external input s range in this mode is 2 V for Irange lt 1 A and 1 V for frange 1 A The polarity is again taken from the American Polarity Convention described in section 2 3 Use the ADD TO SCAN key to toggle adding the external input voltage to internally generated scans or holds This key leaves engaging the control loop lighting the CELL button up to the scan controls Use the DIRECT CONTROL key if potentials or currents to be applied to the cell come only from the external input If the cell is enabled via the CELL button DIRECT CONTROL engages or disengages the control loop taking control voltages or currents solely from the external input The external input is ignored taken as 0 V if both the ADD TO SCAN and DIRECT CONTROL lights are dark 10kQ 50 pF Iwe Irange SRS stanford Research Systems 28 EC301 Potentiostat Galvanostat ZRA 3 Operation
72. ing command sequence produces the waveform shown in figure 33 Slanted text following a command is only used to clarify the example and would be rejected by the EC301 PLINIT Initialize the waveform generator PPOINT 2 The waveform will have 3 control points PSTEPS 200 Baseline potential will increment in 200mV steps Baseline will increment 4 times 100 The zeroth point is at 100mV 500000 The zeroth point is held for 2s PLIMIT 4 PDATAP O PHOLDT O PDATAP 1 400 The first point amplitude is 400mV PHOLDT 1 62500 The first point is held for 250ms PINCRM 1 1 1 The first point is added to the baseline PDATAP 2 100 The second point amplitude is 100mV PHOLDT 2 250000 The second point is held for 1s PINCRM 2 0 O The second point is not added to the baseline and is the last point PLENDM 1 Set the scan to end after the set number of increments PPROGM Load the pulse program verify parameters PSTART Start the scan a a rele 0 8V 0 6V 0 4V Vwe Volts vs reference 0 1V Time Figure 33 Sample normal pulse waveform SRS stanford Research Systems 117 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 4 Programming examples 7 4 2 Cyclic voltammetry The cyclic voltammetry waveform includes a hold and a ramp reversed at a switching potential The following command sequence produces the waveform shown in figure 34 Refer to figure 31 on page 106 for definitions of the potential delay
73. ire triangle shaped waveform Choose the trigger mode MANUAL allows the GO ARM key to trigger the scan while EXTERNAL mode requires the rear panel scan trigger input See section 5 4 on page 61 for a better description of scan triggers in general and section 3 2 6 on page 34 for a description of the rear panel scan trigger SRS stanford Research Systems 50 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 1 Setting scan parameters potentiostat mode ee Time a A CV program and typical I vs E plot using SINGLE scan type and E1 end condition E Open circuit p Es Rate gt Time b A CV program followed by a simulated jump to open circuit using SINGLE scan type and OPEN CIRCUIT end condition The cell potential is uncontrolled when the return ramp finishes Time c A CV program using CONTINUOUS scan type The triangle shaped program continues indefinitely Figure 19 Parameters used to set up a cyclic voltammogram CV SRS stanford Research Systems 51 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 1 Setting scan parameters potentiostat mode 5 1 2 Linear sweep voltammetry LSV Figure 20 illustrates the parameters needed to specify a LSV scan The procedure is as follows i 2 Use the MODE key to select LSV Cycle through the required parameters using SET
74. its remain set until read cleared by the CLS command or until the unit is turned on with PSC enabled Example ESR Returns the Standard Event Status register value 0 gt 255 ESR 5 Returns 0 if bit 5 CME is cleared or 1 if it is set SRS stanford Research Systems 90 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name ESE set or query bits in the Standard Event Enable register Description The ESE i command sets the Standard Event Enable register to the decimal value i 0 255 The ESE i j command sets bit i 0 7 to j 0 or 1 As shown in figure 29 bits enabled in the ESR register via the ESE register set the ESB bit in the status byte The ESE query returns the value 0 255 of the Standard Event Enable Register The ESE i command queries the value 0 or 1 of bit i 0 gt 7 When the instrument sets a bit in the Standard Event Status Register ESR ESE 7 i j described on the previous page and the corresponding bit is set in the Standard Event Enable Register this one by the user bit 5 ESB of the Status Byte STB described on page 96 is set This causes a SRQ if bit 5 in the Status Byte is set Example ESE Returns the register value in decimal format ESE 2 Returns 0 if bit 2 is cleared or 1 if it is set ESE 48 Sets the register value to 48 bits 4 and 5 set ESE 7 0 Clears bit 7 SRS stanford Research Systems 91 EC301 Pot
75. l 123 progrm 0 123 calls for 123mV to be applied to the cell in potentiostat mode If there is no external input voltage the return value of progrm will be 0 123 SRS stanford Research Systems 67 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 3 Control loop commands Name ecmode Set or query the control loop mode Description The control loop can take its feedback from one of three sources resulting in the three modes described below ecnode 1 Potentiostat Galvanostat Zero resistance ammeter ZRA Name clbwth Set or query the control bandwidth Description Set or query the control loop bandwidth Control loop bandwidth clbwth i 100 kHz 10 kHz Name celimt Enables or disables CE voltage limiting mode Description Sending this command is identical to using the front panel ENABLE key in the CE LIMIT group See the description in section 3 1 3 on celimt 7 i page 22 for more information 0 Disable full 30V compliance Enable CE voltage limit set with front panel or celimv command Name celimv Set the CE voltage clamp limits Description The CE limits are symmetric about SIGNAL GROUND For example f the command celimv 1000 will limit the CE voltage to 1V of SIGNAL GROUND celimv i Units 500 501 502 30000 SRS stanford Research Systems 68 EC301 Potentiostat Galvanostat ZRA 7 Remote
76. l error code Description This query only command returns the code corresponding to the most recent system level error While the errmsg command described on page 97 deals with error messages visible on the front panel this query deals with errors output via the remote interface Error codes are decoded with the errdcd query described on this page These errors are cleared by either a front panel button press or a set command errlst Example badcmd badcmd isn t a known command errlst Query the most recent error 114 The error code is 114 errdcd 114 Let s see what error code 114 is Bad remote command Yes that makes sense irange 5 Use a set command to clear the error errlst O The error has been cleared Name errdcd Decode the error code from errlst Description This query only command returns the description of the error code reported by errlst See the errlst query description on the current page for more information errdcd i SRS stanford Research Systems 98 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list INSR Selftest fail 1 Keypress 2 Knob rotation 4 Remote set 8 Current range 16 22 es Fieldcal begin 128 Fieldcal end 256 Fieldcal fail 512 1024 2048 Timebase acquired 4096 Timebase lost 8192 Error for ERRLST 16384 Query refused MESR CE limit 1 E overload 2 loverlosd 4 Aux 1 overload 8 Aux 2 overload 16 Aux 3 overload
77. lbda over and over again to collect data Name getbdp Query the binary data streaming protocol getbdp i Description This query only command is used by host software to interpret streaming binary data This manual documents protocol 2 Binary data streams in from the EC301 least significant bit LSB first and that may cause some confusion with binary hexadecimal converters that operate byte by byte For example if the EC301 wants to send Oxdeadbeef it will send MSB arrives last gt 11011110101011011011111011101111 LSB arrives first and the byte by byte hexadecimal conversion will make this Oxefbeadde You have to reverse the byte order inside each streamed word to recover the correct value SRS stanford Research Systems 82 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 16 bytes v A 4 bytes 1 First 4 bytes data I frame 4 bytes X 4 bytes v 24 bytes Header Fast state bitfields Synchronous ADC data E data Second data frame Last data frame Footer 7 3 Detailed command list Header marker 0x1f Header length 0x10 Packet counter Payload length Reserved Reserved Header checksum Header terminator 0x0d0a r n Temperature Auxiliary ADC 1 Auxiliary ADC 2 Auxiliary ADC 3 E I overload record Reserved Full checksum
78. mode Tt E Time a A LSV program and typical I vs E plot using SINGLE scan type and Ej end condition E Open circuit E E Time b A LSV program followed by a simulated jump to open circuit using SINGLE scan type and OPEN CIRCUIT end condition The cell potential is uncontrolled when the To wait time finishes gt Time c A LSV program using CONTINUOUS scan type The trapezoid shaped program continues indefinitely Figure 20 Parameters used to set up a linear sweep voltammogram LSV SRS stanford Research Systems 53 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 1 Setting scan parameters potentiostat mode 5 1 3 Steps Figure 21 illustrates the parameters needed to specify a step scan The procedure is as follows i 2 Use the MODE key to select STEP Cycle through the required parameters using SET adjusting values using the knob Times are adjusted using the knob for individual fields and the arrow keys described in section 3 1 16 on page 30 to move between the fields shown below Note that the setability is in 4yus steps 00 00 000 000 o o o minutes seconds milliseconds seconds The maximum delay time is 01 07 108860 274 1 counts x 4 us count Setability is 4 us Choose the scan end condition Figure 21 a illustrates the cell potential for the Ej end condition while 21 b shows it for OPEN CIRCUIT I
79. n section 7 3 6 on page 73 5 5 Setting the end of scan condition The EC301 can either retain or release control of a cell at the end of a scan Retaining control may reduce drift in cell characteristics OPEN CIRCUIT between scans while releasing control may reduce stress on the cell amp Select OPEN CIRCUIT to release control or E I to retain control at the E or J setting SCAN ENDS AT SRS stanford Research Systems 61 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 5 Setting the end of scan condition Only OPEN CIRCUIT is allowed as an end condition for HOLD or TIMED HOLD scan modes SRS stanford Research Systems 62 EC301 Potentiostat Galvanostat ZRA 6 Using the EC301 with a frequency response analyzer FRA 6 Using the EC301 with a frequency response analyzer FRA The EC301 can be used with an FRA to perform electrochemical impedance spectroscopy EIS measure ments The FRA supplies the stimulus for these measurements via the external input and measures the cell response via the E and I outputs Figure 27 shows the EC301 used with the Stanford Research Systems SR780 for this purpose For best results especially at high frequency SRS recommends using the rear panel outputs for EIS measurements SR780 Channel 1 Channel 2 Source A BA B Voltage External input Figure 27 Using the EC301 with the SR780 for impedan
80. nd clears the previous ramp program It must be sent before a new ramp waveform is programmed Sending ramprs will stop any running ramp waveforms Use rampst instead to simply stop the waveform without clearing the program SRS stanford Research Systems 108 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name ramppg x Verify the ramp program parameters for ramp type x Description This query must be sent before beginning a ramp with the rampst command It verifies that the parameters necessary for the given ramp type x are specified If one or more of the parameters are missing ramppg x returns an error code see table below If no parameters are missing ramppg x returns Zero ramppg x has the following valid argument range for x Check parameters for this waveform type 0 Cyclic Voltammetry Linear Sweep Voltammetry Infinite Hold ramppg Timed Hold Arm Linear Sweep Voltammetry The ramppg x error code is a bit field defined as follows EU a RA EN ICI Pe Name rampst Start a ramp or hold Description Sending this command will close the control loop if necessary and run the programmed ramp waveform Use rampst 4 or rampst 5 for scans triggered with the rear panel SCAN TRIGGER input rempst i op Bara Vrap 1 ET 5 Arm in preparation for an LSV ramp SRS Stanford Research Systems 109 EC301 Potentiostat Galvanostat ZRA 7 Remote pr
81. nly return bit i Reading the register will also clear it Sending MESR will clear the entire register while sending MESR i will only clear bit i Table 8 lists the conditions corresponding to the register bits Bit Name Set when Bit Name ____________ Setwhen CEL CE limit The CE voltage limit either 30V or the user defined limit was reached E overload the E measurement exceeded 15V 2 IOL I overload the I measurement exceeded 200 of a range or 1A 3 A01 Auxiliary ADC channel 1 overload the BNC input exceeded MESR i 10V 4 Auxiliary ADC channel 2 overload the BNC input exceeded ne 10V Auxiliary ADC channel 3 overload the BNC input exceeded 5 A03 10V ES No remote amplifier EC19 detected CE limit The CE current limit 1A was reached Table 8 The Measurement Status register bits Example MESR Returns the Instrument Status register value 0 gt 65535 MESR 4 Returns 0 if bit 4 CRC is cleared or 1 if it is set SRS stanford Research Systems 94 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name MESE set or query bits in the Measurement Status Enable Register Description The MESE i command sets the Measurement Status Enable register to the decimal value i 0 65535 The MESE i j command sets bit i 0 gt 15 to j 0 or 1 As shown in figure 29 on page 99 bits enabled in the MESR register define
82. ntiostat Galvanostat ZRA References C Major symbols and abbreviations Symbol Meaning Usual units Potential of an electrode versus a v reference SRS Stanford Research Systems 126 EC301 Potentiostat Galvanostat ZRA References Alphabetical command index CLS 97 ESE 91 ESR 90 IDN 86 OPC 86 RST 86 SRE 97 STB 96 TST 86 WAI 86 addscn 66 arbcyc 113 arbdiv 112 arbdly 112 arbend 112 arbget 114 arbpts 112 arbrst 111 arbrun 115 arbset 113 arbtyp 114 autotb 89 avgexp 81 bireje 75 bireji 76 brenab 75 ceenab 70 celimt 68 celimv 68 cellon 70 cicorr 72 cidlay 72 ciopen 71 ciperd 72 clbwth 68 dentrl 67 eadcfl 77 eadcrg 77 ecmode 68 errdcd 98 errlst 98 errmsg 97 exttmb 89 fpgarv 65 getaux 80 getbda 82 getbdp 82 getrtd 116 iadcfl 78 ifcclr 87 S RS Stanford Research Systems ilevel 80 INSE 93 INSR 92 irange 78 irenab 71 irnaut 79 irtype 71 limitg 69 lockfp 87 lpfile 76 lpfili 76 macadr 87 MESE 95 MESR 94 nulcmd 88 pdatap 101 pfback 71 pholdt 101 pincrm 102 plendm 104 plimit 103 plinit 104 plstop 105 polbda 82 ppoint 100 127 pprogm 104 progrm 67 pstart 105 psteps 100 rampcy 110 rampdt 108 rampen 110 ramppg 109 ramppt 106 ramprs 108 ramprt 106 rampst 109 rotate 74 rtdohm 116 scanem 110 scantp 110 scntrg 73 setcu
83. ogramming rampen x rampcy x scantp i scanem i 7 3 Detailed command list Name rampen End the ramp in progress Description This command will end a running ramp waveform without clearing the program Name rampcy Set or query the number of ramp cycles Description The repeating scan unit illustrated in figure 31 can be repeated a few times or forever Use this command to set a finite number of repeats after disabling single scanning with scantp 0 1 2 8 264 Note that sending rampcy 1 will still set the Ez 12 vertex twice since the repeating scan unit will be run once Send scantp 1 to set the single scan type for just one scan Name scantp Set or query the scan type Description This command enables or disables single scanning 0 Continuous scanning A single scan sets the end scan condition after waiting the first T delay shown in figure 31 If this is disabled the scan will continue and repeat the repeating scan unit The number of repetitions is infinite by default but can be made finite by sending a value for rampcy Name scanem Set or query the scan end condition Description Single scans can either return the cell to open circuit or to the Eo Ip vertex shown in figure 31 Scan end condition DIET Hold at Eo Io SRS stanford Research Systems 110 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 18 Ar
84. ogramming 7 3 Detailed command list 7 3 5 TR compensation Name irenab Enable or disable IR compensation Description Enable or disable either mode of IR compensation This corre sponds to pushing the front panel ENABLE key described in section 3 1 12 on re 27 irenab i page Setting 0 Disable IR compensation Enable IR compensation Name irtype Set or query the IR compensation mode Description Set or query the IR compensation mode This corresponds to pushing the front panel MODE key described in section 3 1 12 on page 27 irtype i i ay Setting 0 Current interrupt Positive feedback Name p back Set the positive feedback amount Description No description fback x gt Name ciopen Set or query the CE switch open time for current interrupt Description This command sets or queries the interruption time for current interrupt IR compensation The resolution is 100us This corresponds to the topen delay shown in figure 6 on page 27 us 100 200 300 1 x 10 Is ciopen i The interruption time must be shorter than the time between interrupts Be sure to set a valid value for ciperd after setting ciopen SRS stanford Research Systems 71 EC301 Potentiostat Galvanostat ZRA 7 Remote programming ciperd i cicorr i cidlay i j 7 3 Detailed command list Name ciperd Set or query the interruption frequency for current interrupt Desc
85. on Signal floating ground banana jacks Signal ground ohmically connected to chassis ground Floating ground can float 4 Signal floating ground isolation 10 MQ RTD input 5 pin connector for Pt RTD temperature probe e Raw E output BNC 15V analog output Accuracy 0 2 of VRE VwE SENSE E 5mV Output impedance 500 10mA max output current e Raw I output BNC 2V analog input Accuracy Iwg within 4 Accuracy Iwg within 4 0 5 of Venc x Lange a 0 2 of Venc x Lange a Output impedance 500 10mA max output current e CE 3 output BNC 10V analog output Accuracy 1 of Vor 3 10mV Output impedance 500 10mA max output current S RS Stanford Research S ystems 14 ES V relative to signal ground E 0 2 x Tange 1 A range E 0 2 x Tange other ranges EC301 Potentiostat Galvanostat ZRA General information 1 3 Specifications e Synchronous ADC input Sampled synchronously with E and I ADCs 10V analog to digital input input impedance 100kQ 16 bit resolution e Ethernet interface e IEEE 488 interface e Chassis ground e Power entry module SRS stanford Research Systems 15 EC301 Potentiostat Galvanostat ZRA 1 General information Differential electrometer Input impedance gt 1TQ 20pF Input bias current lt 20pA Common mode rejection ratio CMRR Bandwidth CMRR dB 50 00 07 100 kHz 60 70 typ Bandwidth gt 10MHz Cell c
86. ostat ZRA 1 General information 1 3 Specifications Voltage and current measurement accuracy e Voltage measurement accuracy 0 2 of reading VRE VwE SENSE 5mV e Current measurement accuracy 1 A range 0 5 of reading Iwe a E 0 2 of range e Current measurement accuracy other ranges 0 2 of reading we J e Power amplifier Compliance voltage t 0 2 of range gt 30V full compliance Maximum output current gt t1A Slew rate power amplifier in isolation gt 10V ps Output short circuit protected S RS Stanford Research Systems 7 1 3 Specifications EC301 Potentiostat Galvanostat ZRA 1 General information 1 3 Specifications Potentiostat mode e Applied potential accuracy Potential versus reference within 0 2 of setting 5mV 0 5 of setting 5mV 1 of setting 5mV e Applied potential resolution General potential set with thumbwheel or remote interface 500uV Performing an automatic scan CV or LSV 2004 V e Noise and ripple lt 20UVims 1Hz gt 10kHz e Applied E range 15V versus reference CE lt 30V versus signal ground SRS stanford Research Systems 8 EC301 Potentiostat Galvanostat ZRA 1 General information Galvanostat mode 1 3 Specifications e Applied current accuracy 0 5 of setting 4 0 2 of current range 1 A range 0 2 of setting 4 ZRA mode e Voltage offset CE sense and
87. prt Set or query a ramp rate for the ramp waveform Description As illustrated in figure 31 there are two ramp rates needed to define a ramp waveform 0 ES he i E Galvanostat Tenge 1 2 2000 These rates take multiples of 1004 V s in potentiostat mode and milli fractions of the full scale current Lange per second in galvanostat mode They are always entered as positive numbers The actual scan direction sign of the rate will be determined by the relative magnitudes of the vertices set with ramppt Maximum current on the 1 A range is 1 A but it is fine to scan at 2 A s There is no special restriction for scan rate on the 1 A range For example the command ramprt O 1000 Irange sets the Ro ramp rate to 100mV s potentiostat mode or 48 mode The command in galvanostat ramprt 0 1000 will return the value loaded into index 0 SRS stanford Research Systems 107 EC301 Potentiostat Galvanostat ZRA 7 Remote programming rampdt i Hx ramprs 7 3 Detailed command list Name rampdt Set or query a delay time for the ramp Description As illustrated in figure 31 there are three delay times needed to define a ramp waveform 0 1 2 4294967295 232 1 For example the command will set T to 1s The command returns the value loaded into index 0 rampdt O 10000 rampdt 0 10000 Name ramprs Reset the ramp program Description This comma
88. r 65 setvol 65 stsync 73 trgarm 73 verbmd 87 vfdmsg 88 vlevel 80 EC301 Potentiostat Galvanostat ZRA
89. rent program in galvanostat mode Description This command provides an easy way to control a DC current with out setting up a scan fraction of range For example the sequence ecmode i ceenab 1 irange 4 setcur 0 543 setcur 5 43e 4 will set up a program current of 0 543mA in galvanostat mode The argument to setcur is the signed floating point fraction of the current range Since irange 4 chooses the 1mA range an argument of 0 543 sets a control current of 0 543 x 1mA 5434A The setvol query command will return the actual setpoint in A instead of the fraction of full scale This command is not allowed in potentiostat or zra mode Name addscn Set or query the external input s add to scan mode Description This command enables or disables the external input without af fecting the state of the control loop Setting 0 Voltage at external input ignored Voltage at external input added to scan or hold This is useful for adding a waveform from an external source to a ramp gener ated by the EC301 For example a sine wave could be added to a ramp for AC voltammetry Changing the addscn state will turn the external waveform on or off without affecting the EC301 s waveform If 1V is applied to the external input the sequence ecmode O setvol 1000 ceenab i addscn i will result in OV over the cell SRS stanford Research Systems 66 EC301 Potentiostat Galvanostat ZRA 7 Remote programming
90. ription This command sets or queries the t period described in figure 6 on page 27 This is the time between interrupt cycles set with 1ms resolution ms 1 2 3 10000 The time between interrupt cycles tp must be longer than the interruption time topen Be sure to set a valid value for ciopen described on the preceding page after setting ciperd described on the current page Name cicorr Set or query the correction percentage used for current interrupt IR compensation Description As described in section 3 1 12 on page 27 a fraction of AV is added to the program voltage after current interruptions Sending cicorr 0 will make AV 0 and sending cicorr 100 will make AV AV 712 200 Name cidlay Set or query the voltage sampling times used during current interrupt IR compensation Description This command sets the tg and tae sample delays described in figure 6 on page 27 Both sample delays are entered in integer ps 0 tao open delay Kea tac closed delay Aaah ADS SRS stanford Research Systems 72 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 6 Scan trigger commands Name trgarm Set or query the scan trigger arm condition Description The instrument must be armed before a scan can be started with an external trigger The armed instrument will wait for a trigger edge before scanning This command will set or query this waiting
91. rolled when the return ramp finishes Time c A cyclic current ramp program using CONTINUOUS scan type The triangle shaped program continues indefinitely Figure 23 Parameters used to set up a cyclic current ramp scan SRS stanford Research Systems 57 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 2 Setting scan parameters galvanostat mode 5 2 2 Linear current ramp Figure 24 illustrates the parameters needed to specify a linear current ramp scan The procedure is as follows l Use the MODE key to select LSV While this scan mode is named for its use in potentiostat mode it will set up a linear current ramp in galvanostat mode Cycle through the required parameters using SET and adjust values using the knob Choose the scan end condition Figure 24 a illustrates the cell potential for the J end condition while 24 b shows it for OPEN CIRCUIT Choose SINGLE or CONTINUOUS scanning Single scans illustrated in figures 24 a and b go to the end scan condition after the T wait time Continuous scans illustrated in figure 24 c track back to I after the T wait time with the same rate used for the forward ramp They then repeat the entire program indefinitely Choose the trigger mode MANUAL allows the GO ARM key to trigger the scan while EXTERNAL mode requires the rear panel scan trigger input See section 5 4 on page 61 for a better description of scan
92. running average length Description Sets or queries the number of data points averaged to make a measurement result The averaged number is 2 01373 For example the sequence avgexp 4 will make every measurement returned over the remote interface an average of 2 16 internal measurements Sending avgexp clears the instruments s existing averaged data memory New measurement results won t be accurate until the memory is allowed to refil which takes 30ms Please wait at least 30ms after sending avgexp to ensure that measurement re sults are accurate SRS stanford Research Systems 81 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 12 Streaming data Name getbda Start or stop binary data streaming Description This command is intended for users writing their own data acqui sition software See figure 28 on page 83 for an overview of data packets used for streaming getbda i dd 0 Stop streaming data Start streaming data Name polbda Get a single packet of binary data Description This command is intended for users writing their own data acqui sition software See figure 28 on page 83 for an overview of data packets used for polbda streaming While the getbda command page 82 tells the instrument to start streaming an indefinite number of data packets polbda asks for just one This is useful for polling data acquisition in which the host PC sends po
93. splay in order to accommodate frequency response analyzers FRAs Voltages and currents for 1 ohm resistive cell with CE connected to RE BNC outputs Front panel displays ov ALE TYE TT Te ly INE EE LLO 1V e Potentiostat mode V More anodic oxidizing VOLTAGE 0A HV IHLE tye aya etc WE ILILILILIL gt 0 10 CURRENT ale s a a External Oxidation anodic current input BNC RE has negative sign ID ws CE 3 L 1 3V 1V _ _ PIF TET TA y More cathodic reducing oy L III II Galvanostat mode VOLTAGE v RE ATA s A m 4 alfi ILLALLA J I L A 4 gt 10 aa WE CURRENT 0A m a External Reduction cathodic current 1 3V input BNC has positive sign 4 CE 3 ov Figure 2 The EC301 uses the American polarity convention when applying voltages and currents 2 4 Connecting the EC19 to the EC301 Before you do any electrochemical measurements with the EC301 you must first connect the EC19 2 4 1 Necessary Items In order to connect an EC19 to an EC301 you will need a flat blade screwdriver and the umbilical cable All items except the flat bladed screwdriver were provided in your EC301 shipment Each item is pictured in Fig 3 OTTEIN Figure 3 From left to right EC19 umbilical cable EC301
94. t Galvanostat ZRA 7 Remote programming 7 3 Detailed command list No overloads detected during the last packet E overload record One or more overloads detected during the last packet No overloads detected during the last packet I overload record One or more overloads detected during the last packet Table 5 Bit positions in the E I overload record byte SRS stanford Research Systems 85 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list 7 3 13 Remote interface commands IDN RST TST OPC WAT Name IDN return the EC301 s device identification string Description This query only command takes no arguments and returns the device identification string Name RST Reset the EC301 to its default configuration Description This command sets all modes and settings to their default config urations and values Name TST return the Power on Self Test POST results Description This command has no description Name 0PC Operation complete Description This command is implemented for compatibility with the IEEE 488 standard The original intent was for OPC queries to indicate when a long process was complete The EC301 executes commands as it receives them though and so the 0PC query will be always be processed after the long process finishes These queries will thus always return 1 indicating that all previous operations are complete
95. ther parameters shown in figure 6 are set to the default values shown in table 1 Del valne tp 100 ms 10 Hz ciperd see page 72 200 us ciopen see page 71 cidlay see page 72 Table 1 Default values for current interrupt parameters These values are used when current interrupt is engaged using the front panel SRS Stanford Research Systems 27 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 1 Front panel The current interrupt parameters can be adjusted away from their default values using the remote interface See section 7 4 3 on page 119 for an example FEEDBACK mode Positive feedback IR compensation adds a boost voltage Iwg x Ru to the program voltage where R is the uncompensated resistance parameter Use the SET key in FEEDBACK mode to adjust R The allowed ranges for R in each current range are shown in table 2 1A 0 gt 30 100 mA 0 gt 300 10 mA 0 gt 3002 1 mA 0 gt 3k0 100 uA 0 gt 30k0Q 10 A 0 gt 300 kQ ILA 033M 100 nA 0 gt 30 MQ 10nA 0 300 MQ ind 03 GO Table 2 Allowed Ry ranges for each current range 3 1 13 External input The EC301 can take its control voltage directly from the external EXTERNAL INPUT analog input allowing its use with function generators and fre e e quency response analyzers These control voltages can be used by ADDTO DIRECT themselves or added to internally generated scans SCAN CONTROL 5 In potentiostat mode voltages applied at t
96. tically applied value in V 1V is full scale current brenab 0 Turn off bias rejection bireje 1000 Trying to set a custom nulling voltage remote command error returns an error since rejection has been turned off Name bireje Set or query the amount of E bias rejection Description Sets or queries the amount of bias rejection applied to the front panel VOLTAGE output Accepts an argument in fixed point millivolts The brenab command described on page 75 must be sent before this command can be bireje x used 15000 415000 SRS stanford Research Systems 75 EC301 Potentiostat Galvanostat ZRA 7 Remote programming bireji x lpfile i lpfili i 7 3 Detailed command list Name bireji Set or query the amount of I bias rejection Description Sets or queries the amount of bias rejection applied to the front panel CURRENT output The brenab command described on page 75 must be sent before this command can be used The argument is in floating point and indicates what fraction of full scale current will be rejected fraction of full scale 2 000 gt 2 000 Name lpfile Set or query the front panel E low pass filter status Description No description i Setting No filter 10Hz lowpass Name lpfili Set or query the front panel J low pass filter status Description No description Setting No filter 10Hz lowpass EE SRS stanford Research Systems 76 EC301
97. trated in figures 25 a and b go to the end scan condition after the Tz wait time Continuous scans illustrated in figure 25 c step back to I after the T wait time and repeat the entire step program indefinitely 5 Choose the trigger mode MANUAL allows the GO ARM key to trigger the scan while EXTERNAL mode requires the rear panel scan trigger input See section 5 4 on page 61 for a better description of scan triggers in general and section 3 2 6 on page 34 for a description of the rear panel scan trigger I E O Al 2 ps OT Ta e gt T To l 1 lios gt 0 Ya gt Time Time a A current step program using SINGLE b A current step program followed by a scan type and Ej end condition simulated jump to open circuit using SINGLE scan type and OPEN CIRCUIT end condition The cell current and potential are uncon trolled when the Tz wait time finishes I l O A T To Ta To cco le pit gt i gt lt gt Time c A current step program using CONTINUOUS scan type The rectangle shaped program continues indefinitely Figure 25 Parameters used to set up a step scan SRS stanford Research Systems 59 EC301 Potentiostat Galvanostat ZRA 5 Performing scans using the front panel 5 2 Setting scan parameters galvanostat mode 5 2 4 Current hold Figure 26 illustrates the parameters needed to specify current holds or timed holds These scans must
98. urrent input WE 1 4 Ranges 10 decades 1A to InA Frequency response Serial number and firmware revision Serial number 1 4 Serial number and firmware revision If you need to contact Stanford Research Systems please have the serial number of your unit available The 5 digit serial number is printed on a label affixed to the rear panel the unit is powered on The serial number can also be displayed on the front panel after the unit is powered on by pressing the DISPLAY key Firmware revision The firmware revision code is shown on the front panel when the unit is powered on S RS Stanford Research S ystems 16 EC301 Potentiostat Galvanostat ZRA 2 EC301 basics 2 EC301 basics 2 1 Software The EC301 is intended to operate with the SRSLab Windows software package SRSLab can be downloaded from the SRS web site www thinkSRS com Complete instructions for SRSLab in the form of documentation videos are also available on the website 2 2 Functional block diagram Figure 1 illustrates the major signal paths in the EC301 SRS stanford Research Systems 17 EC301 Potentiostat Galvanostat ZRA nternal scan generation S gt Potentiostat mode External input ea Galvanostat mode Positive feedback level Potentiostat mode Galvanostat mode Program E I output Le 100 CE 3 output
99. ve larger holes on the bottom 2 In each hole is a metal clip Place a small screwdriver into one of the small holes and firmly push it in to the small gap above the clip The screwdriver should go in about half an inch The thickness of the screwdriver shaft pushes the clip down toward the larger hole 3 The larger hole should open up Place a stripped wire into the hole and remove the screwdriver SRS stanford Research Systems 39 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 11 Grounding posts SIGNAL GROUND FLOATING GROUND S RS Stanford Research Systems 3 2 Rear panel These grounding posts should be connected together un less the cell s working electrode is intrinsically grounded Disconnecting these isolates the CE to WE current path from earth ground allowing measurements with grounded working electrodes See section 4 2 for more information on this situation 40 EC301 Potentiostat Galvanostat ZRA 3 Operation 3 2 Rear panel 3 2 12 Raw analog outputs These outputs carry the same signals as their counterparts on the RAW E RAW front panel but without any bias rejection or filtering See section 3 1 10 for a better description of the E and I output voltages The same polarity convention applies to both the front and rear panel outputs OUTPUT OUTPUT The output resistance of these sources is 50Q the same as for those on the front panel The input resistance of whatever these outputs are conne
100. x For example the waveform shown in figure 30 shows four steps The command would make the pulsed waveform either stop or turn around depending on the plendm command Name plendm Set or query the pulsed waveform end mode Description The pulsed waveform can either run in one direction and stop or continuously scan between two endpoints 0 Baseline increment reverses every plimit steps Baseline will increment plimit steps and stop plendm i Name plinit Initialize the pulsed waveform Description This command must be sent before a pulsed waveform can be output See the example pulsed waveform example in section 7 4 1 on page 117 for more information plinit Name pprogm Verify the pulse program has no missing points Description This query must be sent before beginning a pulse waveform with the pstart command It verifies that there are no missing data points for the pulse program If one or more points are missing pprogm returns an error code see table below If no points are missing pprogm returns zero The pprogm error code is a bit field defined as follows E 0 J 1 One or more unique points has no data EJE Po Gt reserved SRS stanford Research Systems 104 EC301 Potentiostat Galvanostat ZRA 7 Remote programming 7 3 Detailed command list Name pstart Start the pulsed waveform pstart Description Sending this command will close the control loop and run the pro

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