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Chapter 1 DECADE II electrochemical detector

Symbols

The following symbol are used on the rear panel and oven compartment of
the DECADE II:

Consult the manual for further safety instructions

Frame or chassis ground terminal

The following pictograms are used in the DECADE II manual:

Caution

Caution, risk of electric shock or other electrical hazard (high
voltage)

Содержание DECADE II 171

Страница 1: ...71 5813333 info AntecScientific com https AntecScientific com Antec Scientific Industrieweg 12 2382 NV Zoeterwoude The Netherlands DECADE II Electrochemical Detector User manual 171 0011 Edition 12 2...

Страница 2: ...demarks of Antec Whatman word and device and Whatrnan word only are trademarks of Whatman lnternational Ltd SOLVENT IFD and AQUEOUS IFD are trademarks of Arbor Technologies Inc Clarity DataApex are tr...

Страница 3: ...materials IEC61010 2 010 2003 2nd ed Immunity 2004 108 EC Electromagnetic immunity EN61326 1 2006 EN61000 4 2 EN61000 4 3 ENV50204 EN61000 4 4 EN61000 4 5 EN61000 4 6 EN61000 4 8 EN61000 4 11 Emission...

Страница 4: ...e disposed as unsorted municipality waste Collection recycling information Please ship the instrument back to the manufacturer Antec Leyden the Netherlands at the end of life time of the product The m...

Страница 5: ...sed on the rear panel and oven compartment of the DECADE II Consult the manual for further safety instructions Frame or chassis ground terminal The following pictograms are used in the DECADE II manua...

Страница 6: ...l should not open the instrument Replace blown fuses with fuses of proper type and rating as stipulated on the rear panel and specified in the installation section of this manual The fuse holder is in...

Страница 7: ...personnel only Use proper eye and skin protection when working with solvents Additional safety requirements or protection may be necessary depending on the chemicals used in combination with this equi...

Страница 8: ...Installation 13 Maintenance 17 DECADE II controller 19 Introduction 19 Overview of DECADE II screens 20 Parameters 24 ALEXYS DECADE II driver 30 Detection and parameters 33 Introduction 33 Internal or...

Страница 9: ...equency 59 Working electrode material 60 References 62 Optimisation of working potential 63 Introduction 63 Electrochemical reactions 63 Hydrodynamic and scanning voltammogram 64 Optimisation using a...

Страница 10: ...g guide 79 No detector response 79 High cell current 79 Noisy baseline 79 Decreased sensitivity low S N ratio 80 Base line oscillations 80 Saturation of output 80 Dummy cell 81 External dummy cell 81...

Страница 11: ...ompartment accommodating column and flow cell This flow cell has surprised researchers for its unsurpassed S N ratio and therefore you now possess the best possible combination for extremely sensitive...

Страница 12: ...12 DECADE II user manual ed 11...

Страница 13: ...the system and inspect it for completeness and for possible damage Contact your supplier in case of damage or if not all marked items on the checklist are included Prior to shipment your detector has...

Страница 14: ...always accessible HPLC connections Use proper eye and skin protection when working with solvents The manufacturer will not accept any liability for damage direct or indirect caused by connecting this...

Страница 15: ...f nitric acid are left in the tubing or pulse dampener check with pH paper Flush the system with HPLC buffer If an ISAAC reference electrode is used make sure that the buffer contains 2 mmole l chlori...

Страница 16: ...the cell cable is not correctly connected the cell is only partly or not at all filled with buffer the outside of the flow cell is wet particularly the part between the auxiliary and working electrode...

Страница 17: ...sewage system This instrument has a lithium battery inside Replacement of the battery should be performed by qualified service personnel Dispose the battery according to chemical waste only Replace bl...

Страница 18: ...18 DECADE II user manual ed 11...

Страница 19: ...of appearance The nature of an item can be 1 Control parameters with a cursor box can be attained via cursor buttons and changed by the value button 2 Status without a cursor box a parameter reflects...

Страница 20: ...0 5 0 V S T A T F i l t 0 0 2 H z C o m p o f f 2 5 3 0 C 2 1 1 2 0 P R E V C E L L O N M A R K A Z E R O N E X T if ID 1 1 D I c 2 3 4 5 n A 4 P I c 1 5 0 m A S T A T 91 2 P I c 1 2 0 6 n A 5 S I c 6...

Страница 21: ...4 5 A P U L S E 1 17 R a n g e 5 A F i l t 0 0 2 H z t 5 0 0 m s S T A T E 1 0 1 0 V C o m p o f f 3 0 3 1 C 2 1 1 3 7 P R E V C E L L O N M A R K A Z E R O N E X T if ID 1 1 D I c 2 3 4 5 n A 4 P I...

Страница 22: ...0 0 5 7 V I c 2 3 4 5 A S C A N 1 23 R a n g e 5 0 A C y c c o n t E 1 0 2 0 V S T A T O f f s 1 0 3 0 3 0 C E 2 1 2 0 V P R E V S T A R T C E L L O N N E X T if ID 1 1 D I c 2 3 4 5 n A 4 P I c 1 5...

Страница 23: ...E S C A N D I A G D I A G 26 P R E V N O I S E K E Y B D I S P L F W D I S P 28 P R E V B o o t v e r s i o n 1 2 1 F W 68 F i r m w a r e v e r s i o n 1 7 2 C h e c k s u m 2 1 0 8 2 3 9 6 P R E V K...

Страница 24: ...see page 30 Control Comp off changes to Comp on If cell current exceeds the max compensation a message cell current exceeds max compensation appears In that case max compensation will be applied whic...

Страница 25: ...o E1 continuously Pressing STOP or finishing the cycle sets the potential to E1 C Cycles events setup Controls the number of times a time file has to be repeated This number can be 1 999 or continuous...

Страница 26: ...tup dc stat prog Filter settings 0 5 to 0 001 Hz cut off frequency in 1 2 5 steps C Filt run Reflects the actual filter setting S Firmware system Displays firmware version S Hold resume run scan stat...

Страница 27: ...offset can be set between 50 and 50 C Offs run Displays percentage offset during execution of a time file S Outp prog Control of four output functions in EVENTS Is open high if 0 is closed low if 1 A...

Страница 28: ...this run cycle counter Cy is reset to 1 STOP also deactivates the outputs Aux 1 and 2 and Relays 1 and 2 status 0000 and sets the electric valve to load if present F t pulse setup2 pulse stat Displays...

Страница 29: ...an be set between 20 and 100 ms in 20 ms increments C Tsensor system Displays active temperature sensor S Valve prog Controls the electrically actuated injector during execution of a time file Forces...

Страница 30: ...s that timed events are not executed from time files but from the events page in ALEXYS software DECADE II time files are not supported in ALEXYS data system Use events page instead Fig 10 DECADE II d...

Страница 31: ...E II controller 31 A unique feature of ALEXYS data system is the scanning voltammetry module From the DECADE II device driver window all parameters are set The so called scan shell is opened and the s...

Страница 32: ...32 DECADE II user manual ed 11...

Страница 33: ...o an oxidation or reduction reaction The resulting electrical current is amplified by the current potential I E converter Fig 11 Fig 11 DECADE II signal processing from electrochemical flow cell to ou...

Страница 34: ...same time base Serial mode detection is especially suitable for OX RED or RED OX applications examples are analysis of vitamin K and nitro tyrosine using micro HPLC The first flow cell is a reactor ce...

Страница 35: ...T 03 flow cells for parallel detection Navigation in dual cell menu All menus for a dual flow cell system are similar to a single cell system with 2 exceptions First in the top right corner a number i...

Страница 36: ...nu Range Range selection is done in the SETUP or STAT screen in DC PULSE and SCAN mode A number of ranges can be selected the maximum current that can be compensated for using auto zero and offset dif...

Страница 37: ...2 A 25 A 200 pA 250 25 nA 1 A 25 A 100 pA 25 nA 500 nA 25 A 50 pA 25 nA 200 nA 25 A 20 pA 25 nA 100 nA 25 A 10 pA 25 nA 50 nA 2 5 A From firmware 3 00 the noise level in ranges 200 500 pA and 1 nA ha...

Страница 38: ...output can be inversed Oxidative and reductive analyses generate opposite currents For data acquisition traditionally chromatographic peaks have a positive amplitude Therefore selection of polarity i...

Страница 39: ...n we will look at peak width filter settings cut off frequency amplitude response plots and finally at a few chromatograms before and after applying ADF Frequency A scientific definition of frequency...

Страница 40: ...to determine this frequency is the same The duration of the full peak is measured and expressed in Hz Fig 20 Frequency tells how often something happens 1 peak in about 0 25 min 15 s f 1 15 0 07 Hz 4...

Страница 41: ...01 Hz which corresponds to 10 100 s peak width Fig 22 Typical chromatogram with peak widths between 10 100 s Noise in chromatography can come from different sources Pump pulsations are typically shown...

Страница 42: ...uired signal Traditionally in many detectors for chromatography an analogue low pass filter is applied rise time filter A passive RC filter consists of resistors and capacitors An active higher order...

Страница 43: ...tics behind the signal processing routine Well known names in this field are Bessel Chebychev Savitsky Golay Hamming and many others Amplitude response plot There are several ways to describe the filt...

Страница 44: ...f poles In a hardware filter the number of poles is the number of filter circuits that are placed in series Fig 26 Analogue 6 pole Bessel filter A digital filter does not have poles but it is characte...

Страница 45: ...oise S N ratio No matter how advanced a filter is it is only possible to apply low pass filtering if noise frequencies are higher than the frequency of the signal Fig 27 From top to bottom filter sett...

Страница 46: ...peak width a 0 05 Hz filter setting is advised If peaks are 50 s a 0 01 Hz filter is advised to start with Note that if a chromatogram has interesting peaks of 10 s as well as 50 s it may not be poss...

Страница 47: ...requency noise is suppressed remaining noise components will be in the same frequency range as chromatographic peaks As suppressing noise will always result in some suppression of signal it is advised...

Страница 48: ...48 DECADE II user manual ed 11...

Страница 49: ...E II output contacts to control the status of external equipment Table IV A time file used for offset programming at 5 00 min time range filt valve auto zero output offset E cell id 00 00 1 nA 0 5 Hz...

Страница 50: ...Scroll to Time 0 00 min and press DEL Answer Yes to the question 4 Programming the time file is done by entering all parameters for Time 0 00 and pressing ADD This is repeated for each time line in Ta...

Страница 51: ...s the inject marker on connector B The contact is high when the valve is in load position and low in the inject position It can be used to start the integration software when injection is done Overloa...

Страница 52: ...nd 2 default or 3 Activated by time file Outp 0100 4 5 6 Relay 2 Out Contact between 4 common and 5 default or 6 Activated by time file Outp 1000 7 Cell on In Trigger to switch on cell 8 Reset In Rese...

Страница 53: ...ector C high load low inject 14 To I Out Forces electric injector to inject 15 To L Out Forces electric injector to load Outputs 4 7 12 14 and 15 are level triggered Level triggered TTL input contacts...

Страница 54: ...54 DECADE II user manual ed 11...

Страница 55: ...ode WE is regenerated at a frequency of 0 5 3 Hz by the application of a series of potential changes This is particularly useful for certain applications where the working electrode is rapidly fouled...

Страница 56: ...he AUX and result in an increase of the noise Cleaning the AUX electrode with metal wool is a way to remove this coating Be careful NOT to touch the working electrode with metal wool 5 Reference elect...

Страница 57: ...potential This monolayer is electrochemically removed from the electrode surface during time interval t3 by applying a negative potential Optimisation of wave forms LaCourse and Johnson 2 4 have publ...

Страница 58: ...s of the AC power supply Until a certain limit increasing ts will result in an increase of signal A limiting factor is the accumulation of adsorbed species at the working electrode that attenuate the...

Страница 59: ...tor frequency There are two important considerations with respect to integrator frequencies applied in HPLC If the frequency is too low data will be lost and artefacts may be introduced If the frequen...

Страница 60: ...ulse mode is illustrated in Fig 34 When the potential is changed a large charging current is detected Fig 34 peak 1 3 and 5 followed by a stabilisation of the current Fig 34 part 2 4 and 6 The output...

Страница 61: ...current of the noble metals gold Au and platinum Pt is stabilised faster than the cell current of glassy carbon GC due to a much lower capacitance of the noble metals For Pt and GC the negative peaks...

Страница 62: ...Pulsed amperometric detection of carbohydrates amines and sulphur species in ion chromatography the current state of research J Chromatogr 640 1993 79 96 2 D C Johnson en W R LaCourse LC with pulsed...

Страница 63: ...Electrochemical reactions In electrochemical detection ECD a reaction of the analyte at an electrode surface is monitored This distinguishes ECD from most other detection techniques where detection is...

Страница 64: ...rnative for the chromatographic construction of an I E relationship is the application of scanning voltammetry The working potential runs between two pre set values and the current is measured while t...

Страница 65: ...nt However at higher working potentials more analytes are detectable So as to selectivity a low working potential will be favourable Working at a potential on the slope of the I E curve will result in...

Страница 66: ...d to a better detection A constant temperature is of paramount importance for a stable baseline and reproducible detection conditions Fig 38 Selectivity in LC EC of compound X and Y is optimised by ch...

Страница 67: ...completely and the signal decreases rapidly This means that the flow rate not only affects temporal peak width and analysis time but also peak height Also the background signal is sensitive towards fl...

Страница 68: ...and step 2 to 4 is repeated until the lowest potential setting Fig 40 5 The peak heights and the background currents are plotted against the working potential Fig 36 The working potential which gives...

Страница 69: ...10 100 mol l When the analyte is already in solution it should be diluted in HPLC buffer until the desired concentration 3 An injection loop of 100 l is installed and the LC flow rate is set at 40 l...

Страница 70: ...range is set at 5 A A scan speed of 10 mV s is selected 7 The analyte is injected and the scan is started by pressing the START in the SCAN STAT screen of the DECADE II at the time the analyte plug en...

Страница 71: ...CHAPTER 8 Optimisation of working potential 71...

Страница 72: ...72 DECADE II user manual ed 11...

Страница 73: ...instrument control data acquisition at 1 2 5 and 10 Hz Injector sensor Starts system clock at injection Oven height 37 cm from 7 C above ambient to 45 C accuracy 0 5 C stability 0 1 C accommodates co...

Страница 74: ...auto zero offset valve position if present and E cell Rear panel I O connections Mains Output 2 Connectors 15 pins A B manual valve C RS232C connector Physical specifications Dimensions 44 D x 22 W x...

Страница 75: ...rror Please contact your local supplier if one of the above errors occur Furthermore the following messages can be displayed on the LCD screen during a measurement Table XI Messages Message Advice 01...

Страница 76: ...76 DECADE II user manual ed 11...

Страница 77: ...comprise cell potential range auto zero offset filter electrical injector and control of DECADE II output contacts for control of external equipment During operation a remote screen is shown and the...

Страница 78: ...8 DECADE II user manual ed 11 The manufacturer will not accept any liability for damage direct or indirect caused by connecting this instrument to devices that do not meet the relevant safety standard...

Страница 79: ...not recycle the buffer High WE potential Optimise potential if possible use smaller WE diameter Salt bridge in REF not saturated Refill with wetted KCl crystals Retained peaks from previous runs Wait...

Страница 80: ...seals valves Over tightened cell bolts Adjust cell bolts check pump pressure Air bubbles in cell or REF Maintenance REF Temperature oscillations Set oven temperature Contaminated buffer high Icell Re...

Страница 81: ...are due to the tolerance of the resistor 1 The capacitor functions as a noise generator and in fact resembles the capacitance of a well functioning VT 03 flow cell in an ideal HPLC set up The noise ge...

Страница 82: ...rnal dummy cell can be measured at the output As with the external dummy cell the noise should be better than 2 pA Detector settings in the NOISE screen are the same as in Table XII with exception of...

Страница 83: ...ry for complete listing Table XIII Accessories electrochemical detector Part number Component 250 0040 External dummy flow cell 250 0107 Column clamp 12 mm 250 0113 Fuse 2 5 AT 250 V 250 0122 RS232 ca...

Страница 84: ...84 DECADE II user manual ed 11 Index...

Страница 85: ...tector 17 Common I O contact 52 53 compensation 36 cut off frequency 44 DC mode specifications 73 degassing mobile phase 15 digital filter 42 DSP 43 dual flow cell control 33 dual flow cell navigation...

Страница 86: ...6 58 68 73 79 noise filters 42 offset 37 output frequency 59 pulse mode 59 Overload I O contact 51 52 passivation with nitric acid 15 polarity 38 potential optimisation 63 pulse mode characteristics 5...

Страница 87: ...art I O contact 52 Status I I O contact 53 Status L I O contact 53 t1 control 28 Tefzel rotor 56 timefile 49 example 49 To I I O contact 53 To L I O contact 53 to pos I L I O contact 52 troubleshootin...

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