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Antec DECADE Elite User Manual

Electrochemical detector
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Antec
Industrieweg 12
2382 NV Zoeterwoude
T he Netherlands
DECADE Elite
User Manual
175.0010, Edition 2, 2015
T +31 71 5813333 | F +31 71 5813334 | info@myantec.com | www.myantec.com

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  • Page 1 Antec Industrieweg 12 2382 NV Zoeterwoude T he Netherlands DECADE Elite User Manual 175.0010, Edition 2, 2015 T +31 71 5813333 | F +31 71 5813334 | info@myantec.com | www.myantec.com...

  • Page 2: 175_0010 - Decade Elite User Manual - Rev

    (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from the copyright of the owner. Antec reserves the right to make changes to the design and specifications of the instrument and this manual without prior notice.
  • Page 3 Declaration of conformity We Antec Leyden B.V., Zoeterwoude, The Netherlands, declare that the product: type 175 and 176 DECADE Elite™ Electrochemical Detector to which this declaration relates, is in conformity with the following CE directives: Low Voltage Directive ( 2006/95/EC)

  • Page 4: Table Of Contents

    175_0010 - DECADE Elite user manual - rev 02 Table of contents Table of contents 4 Warning Symbols 7 Safety instructions 9 Introduction 13 Instrument description 14 Installation 17 Site Preparation Requirements 17 Unpacking 18 Mains connection 20 PC connection 21...

  • Page 5: Chapter 1 Table Of Contents

    CHAPTER 1 Table of contents Intended use The DECADE Elite Electrochemical Detector is used in combination with (Ultra) High Performance Liquid Chromatography for the electrochemical detection of suitable analytes in liquid samples. With this technique the amount of electroactive substances in mobile phase can be quantified. The...

  • Page 6: Decade Elite User Manual - Rev

    175_0010 - DECADE Elite user manual - rev 02 WEEE directive All equipment of Antec Leyden which are subjected to the WEEE directive shipped after August 13, 2005 are compliant with the WEEE marking re- quirements. Such products are labelled with the “crossed out wheelie”, de- picted on the left site.

  • Page 7: Warning Symbols

    CHAPTER 1 Table of contents Warning Symbols The following symbols are used in this guide: This sign warns about the risk of electric shock. It calls attention to a procedure or practice which, if not adhered to, could result in loss of life by electrocution. Do not pro- ceed beyond a danger sign until the indicated conditions are fully understood and met.
  • Page 8 175_0010 - DECADE Elite user manual - rev 02 The attention sign signals relevant information. Read this information. The note sign signals additional information. It provides advice or a suggestion that may support you in using the equipment.

  • Page 9: Safety Instructions

    Make sure power cords are connected to correct voltage sources: grounded AC power source, line voltage 100 – 240 VAC. The in- strument should be connected to a protective earth via a ground socket. The DECADE Elite must only be used with appliances and power sources...
  • Page 10 175_0010 - DECADE Elite user manual - rev 02 with proper protective grounding to prevent damage through build-up of static electricity. The power source should exhibit minimal power transients and fluctuations. If necessary connect to a filtered mains socket. USE ONLY WITH 250 V FUSES...
  • Page 11 Always wear protective And gloves when handling toxic or biologically infectious samples to pre- vent bio hazards or hazards while working with the DECADE Elite. If nec- essary the instrument must be decontaminated before decommissioning or shipment of the instrument for repair to Antec or its representatives.
  • Page 12 175_0010 - DECADE Elite user manual - rev 02...

  • Page 13: Introduction

    PULSE mode. Furthermore, a Service, Diag(nostics) and Config(ura- tion) mode are available. In addition, crucial parameters can be controlled by either relays or TTL. The DECADE Elite can support up to 4 flow cells (optional), which makes it possible to perform 4 independent measure- ments with one detector.

  • Page 14: Instrument Description

    175_0010 - DECADE Elite user manual - rev 02 Instrument description DECADE Elite – Front side Description Description Instrument housing '+' and '-' value keys LC tubing inlet/outlet Cursor keys Instrument door panel Door handle (for opening door) 4 x 40 Ch LCD display Function keys <Enter>...
  • Page 15 CHAPTER 1 Introduction DECADE Elite – Back side Description Description Instrument rear panel USB connector (USB B) Type label (pn, sn etc.) Fuse & power rating Digital I/O connector (25-pins sub-D fem) Mains switch/inlet Analog data (9-pins sub-D fem) Grounding stud...
  • Page 16 175_0010 - DECADE Elite user manual - rev 02 DECADE Elite – Oven compartment Description Description Cell cabinet Column clamp Cell connector (9-pins sub-D fem) Mounting hole for cell clamp (M4) Top fan heater (intake) Bottom fan heater (exhaust) Door sensor Mounting hole for column clamp (M3) Mounting plate (for cells &...

  • Page 17: Installation

    Free USB port (required for FW updates) Microsoft Windows 7 Operating System or higher  Detailed requirements for use of the DECADE Elite in combination with Clarity chromatography software are listed in document 195.7000 Com- puter requirements which can be downloaded from the Antec website (www.myantec.com).

  • Page 18: Unpacking

    175_0010 - DECADE Elite user manual - rev 02 For optimum analytical performance it is recommended that the ambient temperature of the laboratory be between 20-25 °C and be held constant to within ± 2 °C throughout the entire working day. Note: that...
  • Page 19 - flow cell(s)* User manual(s) is (are) included on USB stick *) Note that flow cells are not part of the DECADE Elite detector and have to be ordered separately. To unpack the DECADE Elite, lift it from its box by both hands (Fig. 1).

  • Page 20: Mains Connection

    5 cm from the DECADE Elite , if objects are placed at only one side of the instrument and 10 cm from the DECADE Elite, if objects are placed on more than one side of the instruments.

  • Page 21: Pc Connection

    255.255.255.0. Gateway and DNS are not filled in. The instrument is standard delivered with a special crossover LAN (UTP) cable (pn 250.0170) which is part of the DECADE Elite accessory kit (pn 175.0200). If the instrument is delivered as a part of a complete ALEXYS (U)HPLC-ECD system an additional LAN connectivity kit (pn 250.0180)
  • Page 22 175_0010 - DECADE Elite user manual - rev 02 2. Open the menu 'Change adapter settings' on the left panel of the 'Open Network and Sharing Center' window. 3. Right click on the Local Area Connection icon of the LAN card in your...
  • Page 23 8. Connect the other end of the crossover LAN (UTP) cable to the LAN port on the rear panel of the DECADE Elite as depicted on the photograph. 9. Switch on the DECADE Elite. Set the detector temperature to 35°C if a Performance Qualification (PQ) will be executed, or set it to the tempera- ture at which your application is running.

  • Page 24: Software

    175_0010 - DECADE Elite user manual - rev 02 Fig. 3. Example of LAN connection between PC and DECADE Elite. A di- rect connection requires the special crossover UTP cable. With a switch any regular UTP cable can be used.
  • Page 25 Elite Dialogue and Clarity users must have read/write access to all software folders and subfolders. Elite Dialogue To install the software: Download the latest version of the Elite Dialogue from the Antec  website www.myantec.com (register to get access).
  • Page 26 175_0010 - DECADE Elite user manual - rev 02 When a DECADE Elite is available it is automatically detected and  the IP address is shown in the port settings box. If not press port scan or type in the default IP address 192.168.5.1.
  • Page 27 CHAPTER 2 Installation The detector set-up menu will open (see figure on the next page).  Select LAN communication (checkbox) and fill in the IP address 192.168.5.1.  By clicking ‘Auto detect’ the instrument will be automatically connected and the number of available sensor boards shown. ...
  • Page 28 2 or 3 use pin 22 (start 2) and pin 23 (start 3) re- spectively. Add the DECADE Elite device to the Clarity instrument by clicking  the right arrow button (encircled) and select Ext. Start. Dig. Input ‘Device DECADE Elite, Number 1’...

  • Page 29: Hplc Fluid Connections

    HPLC fluid connections In this section the installation & priming of all relevant fluidic connections are described to be able to use the DECADE Elite for the analysis of sub- stances with (U)HPLC-ECD. When working with HPLC solutions and mo- bile phases take the following precautions: Use proper eye and skin protection when working with solvents.
  • Page 30 Valco nuts and ferrules, for Rheodyne valves use Rheodyne valves etc. The use of unsuitable connectors may lead to damage of the parts or the introduction of dead volumes. In case the DECADE Elite was purchased as a part of an ALEXYS HPLC-ECD analyzer, the instrument is...
  • Page 31 CHAPTER 2 Installation If L is too short, this may result in: Leakage   Dead volume at the end of the ferrule (a ‘mixing chamber’). Every ferrule type needs an appropriate length of tubing for connecting it to the type of connection port, depending on the depth of the connection port. Refer to the information provided by the manufacturer for specific infor- mation.
  • Page 32 175_0010 - DECADE Elite user manual - rev 02 However at higher working potentials (typically > 1.2 V vs. salt bridge AgCl ref) also EDTA can become electrochemically active and is not recom- mended. In that case only a passivation step with 15% HNO is recom- mended (see installation guide).
  • Page 33 VALVE connector on the rear panel of the instrument to enable INJECT/LOAD functions. This presence of this valve is automatically detected and no further configuration has to be performed. Fig. 4. Installation of flow cell and column in the DECADE Elite.
  • Page 34 See figure 11 on the next page for reference. Connect the flow cell to the corresponding cell connector in the oven compartment. All cell connectors are marked with a label for identification. In case of a DECADE Elite...
  • Page 35 CHAPTER 2 Installation SCC connect the flow cell to the cell connector on the left side marked “Cell 1”. The cell connector inside the oven compartment is ESD sensitive. Make sure that the flow cell is OFF when removing or connecting the cell cable.
  • Page 36 A/D device. Your system is now ready for use. The DECADE Elite has been developed for continuous operation. For maximum stability it is advised to leave the system ON continuously. If preferred, the flow cell may be switched OFF at...

  • Page 37: Maintenance & Shutdown

    CHAPTER 3 Maintenance & Shutdown C H A P T E R Maintenance & Shutdown Maintenance In this paragraph all maintenance is described which can be performed by the end-user, all other maintenance & service procedures may only be per- formed by authorized service engineers only.
  • Page 38 175_0010 - DECADE Elite user manual - rev 02 Cleaning In general, the DECADE Elite needs very little maintenance. The outside of the detector may be cleaned with a non-aggressive cleaning liquid. Do not use any organic solvents to clean the exterior of the detector, because this may lead to damage of the paint layer.

  • Page 39: Shutting Down The System

    CHAPTER 3 Maintenance & Shutdown Shutting down the system There are a couple of steps to take to switch off an LC system with electro- chemical detector for a longer period of time. Shutting down is not different from most other HPLC systems. Perform the following procedure: ...
  • Page 40 175_0010 - DECADE Elite user manual - rev 02...

  • Page 41: Decade Elite Controller

    Fig. 6. DECADE Elite keyboard. The cursor is on ‘Range’ which allows changes using the value buttons ‘+’ and ‘-’. The ‘Enter’ button is only used to confirm changes in potential (Ec) and range.

  • Page 42: Overview Of Decade Elite Screens

    175_0010 - DECADE Elite user manual - rev 02 Overview of DECADE Elite screens DC mode...
  • Page 43 Chapter 4 DECADE Elite controller Pulse mode...
  • Page 44 175_0010 - DECADE Elite user manual - rev 02 SCAN mode V o u t = + 0 . 0 5 7 V = + 2 3 . 4 5 n A S C A N R a n g e =...
  • Page 45 Chapter 4 DECADE Elite controller CONFIG menu A n t e c M A I N D E C A D E E L I T E D e t e c t o r 1 . 0 0 C O N F I G >...
  • Page 46 175_0010 - DECADE Elite user manual - rev 02 DIAG menu A n t e c M A I N D E C A D E E L I T E D e t e c t o r 1 . 0 0 C O N F I G >...

  • Page 47: Parameters

    Chapter 4 DECADE Elite controller Parameters Explanation: Type S is status, F is function and C is control. Parameter Screen Description Type 28 > 30˚C dc stat Displays the actual (left value) pulse stat and the pre-set oven temperature scan stat (right value).
  • Page 48 175_0010 - DECADE Elite user manual - rev 02 Parameter Screen Description Type means that the cell potential runs from E1 to E2 and back to E1 continuously (/\/\/\/\……..). Press- ing “STOP” or finishing the cycle, sets the potential to E1.
  • Page 49 Chapter 4 DECADE Elite controller Parameter Screen Description Type ID1 master config Sets sensor board 1 as master. When this setting is set to ‘yes’ all parameter settings from sensor board 1 are automatically cop- ied/transferred to all other sensor boards present.
  • Page 50 175_0010 - DECADE Elite user manual - rev 02 Parameter Screen Description Type P12(C-ON) Programmable input: can be con- figured that only cell 1, 2 or 3 is switched ON when active, or ALL cells. P15(C-OFF) Programmable input: can be con-...

  • Page 51: Clarity Decade Elite Control Module

    Vout source config Sets the output source from the analog data output: DAC (pro- cessed digital signal after 16-bit AD conversion) or I/E (true ana- log signal from the I/E converter) Clarity DECADE Elite control module...
  • Page 52 Full control and data acquisition of the DC and Pulse measurement mode is supported in the Clarity chromatography software. Fig. 8. DECADE Elite method window in Clarity. On the main tab the main measurement conditions can be set/controlled (measurement mode & po- tential settings).
  • Page 53 Chapter 4 DECADE Elite controller...
  • Page 54 175_0010 - DECADE Elite user manual - rev 02...

  • Page 55: Detection And Parameters

    200 µA down to 10 pA full scale, without being lim- ited by electronic noise. For this reason the DECADE Elite is equipped with a 24-bit ADC and 16-bit DAC for analogue data output. One of the...
  • Page 56 175_0010 - DECADE Elite user manual - rev 02 panel connected to a recorder or an external A/D converter. Fig. 9. Schematic representation of an electrochemical cell with a three- electrode configuration. Essentially, for the oxidation or reduction reaction it would be sufficient to use only two electrodes.

  • Page 57: Internal Organization

    By using this architecture it is possi- ble to extend the functionality of the DECADE Elite to more than one flow cell by simply adding a sensor board. The control board and other hard- ware is prepared for more than one sensor board.
  • Page 58 2 is a SenCell for detection. Channel 1 and 2 use the same time base of system 1. Parallel mode detection In parallel mode 2 HPLC systems are used with 2 flow cells. In fact, the DECADE Elite is operated as if 2 independent detectors are in one hous- ing.
  • Page 59 Fig. 12. Typical configuration for parallel mode detection. Two independent HPLC systems with dual channel support from OR 110, DECADE Elite and Clarity software. Fig. 13. DECADE Elite with 2 columns and 2 SenCell 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.
  • Page 60 I c = + 2 . 6 6 5 n A 3 5 > 3 5 ° C P R E V Fig. 14. DECADE Elite main menu (top) with active cell indicator in top right corner. Multi-STAT screen showing cell 1 (DC mode) and cell 2 (PULSE mode).
  • Page 61 Chapter 5 Detection and Parameters ranges, and maximum compensation at the less sensitive ranges. This is an inevitable consequence of the tremendous dynamic range that is cov- ered by electrochemical detection. Table II. DC ranges and maximum compensation. Range FS Max comp Range FS Max comp 200 µA 2.5 mA...

  • Page 62: Filter

    Fig. 16. Signal to noise ratio is improved using a filter (A vs. B). The DECADE Elite is equipped with ADF (Advanced Digital Filter) as a tool to filter the acquired signal and improve the sensitivity of the analysis (Sig- nal-to-noise ratio).
  • Page 63 Chapter 5 Detection and Parameters Table IV. DC mode filter setting and corresponding data rate. Filter setting DC mode (Hz) Data rate (Hz) 100(default), 50, 20, 10, 5, 2, 1 2, 1 0.5, 0.2, 0.1 0.05 0.02 0.01, 0.005, 0.002, 0.001 Filter OFF is also a special case.
  • Page 64 175_0010 - DECADE Elite user manual - rev 02...
  • Page 65 To fur- ther improve these detection limits the Antec engineers have developed ADF (Advanced Digital Filter) and the DECADE Elite has been equipped with it as a standard. The improvement factor in signal-to-noise (S/N) ratio depends on the frequency relation of signal and baseline noise.
  • Page 66 175_0010 - DECADE Elite user manual - rev 02 400000 300000 200000 100000 -100000 -200000 -300000 -400000 Fig. 17. Example of a signal with regular evenly spaced alterations: a sine. 400000 300000 200000 100000 -100000 t (min) -200000 -300000 4.15 4.56...
  • Page 67 Chapter 5 Detection and Parameters This is further illustrated by an overlay of the same chromatographic peak with a sine of 0.07 Hz (Fig. 20). 540000 440000 340000 240000 140000 40000 Fig. 20. Overlay of a chromatographic peak with 0.07 Hz sine. Typically in chromatography narrow peaks are in front of a chromatogram while peaks with longer retention times get wider.
  • Page 68 175_0010 - DECADE Elite user manual - rev 02 noise has a more random character. This is illustrated in Fig. 22 where a noise trace is shown with an overlay of a 10 and 0.4 Hz sine. sine f = 10 Hz sine f = 0.4 Hz...
  • Page 69 Chapter 5 Detection and Parameters form a running average filter takes the average of n data points to create a new data point. For example in a 5-points running average filter output data point y[80] is calculated from measured data points x[80] – x[84] as: Each input data point has the same weighting factor of 1/5.
  • Page 70 175_0010 - DECADE Elite user manual - rev 02 between 0 – 1 Hz completely pass while frequencies of higher than 1 Hz are completely blocked. In practice filters behave a bit different from the ideal situation. Amplitude response plot shows a more gradual attenuation profile at higher fre- quency.
  • Page 71 Chapter 5 Detection and Parameters A digital filter does not have poles, but it is characterized by the number of input data points used to calculate a new output data point. For example a 9-point digital filter (Savitzky-Golay) is given as: Y[1] = -0.090909091 X[1] + 0.060606061 X[2] + 0.168831169 X[3] + 0.233766234 X[4] +...
  • Page 72 175_0010 - DECADE Elite user manual - rev 02 Applying ADF in chromatography If noise frequencies in LC-EC differ from the frequency of the signal, noise can be suppressed. Using the right filter setting (cut-off frequency) will spe- cifically attenuate noise and improve the signal-to-noise (S/N) ratio. No matter how ‘advanced’...
  • Page 73 This is particularly difficult if the frequency of the signal is close to the frequency of the noise. The DECADE Elite has a number of filter settings to optimize for best pos- sible signal-to-noise ratio. The width of the peaks of interest is important because wider peaks allow stronger filter settings simply because of the lower frequency of such peaks.
  • Page 74 175_0010 - DECADE Elite user manual - rev 02 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 to switch the DECADE Elite to the highest acceptable sensitivity.

  • Page 75: Introduction

    Chapter 5 Detection and Parameters C H A P T E R Pulsed Amperometric Detection (PAD) Introduction In pulsed amperometric detection (PAD) the working electrode (WE) is re- generated at a frequency of 0.5 - 3 Hz by the application of a series of po- tential changes.
  • Page 76 175_0010 - DECADE Elite user manual - rev 02 Pulse vs. DC mode The pulse mode is quite different from the DC mode. Instead of a constant potential, a series of potential steps is applied in a cyclic manner. The sig- nal is sampled during a fraction of the total pulse cycle.
  • Page 77 Chapter 5 Detection and Parameters (19.2 mol/l). NaOH pellets are not recommended because of their high content. Organic modifiers (acetonitrile) strongly attenuate the signal of most carbohydrates in PAD and are therefore not recommended. Pulse settings In PAD of carbohydrates a series of potentials is applied in a continuous cyclic manner.
  • Page 78 175_0010 - DECADE Elite user manual - rev 02 steps and 6 time settings, may lead to a time-consuming optimization pro- cedure. In practice, the pulse mode is more straightforward and published in several excellent review papers and application notes.
  • Page 79 Chapter 5 Detection and Parameters based on formation and removal of a (metal-) oxide layer. This is impossi- ble with glassy carbon. References 1. D.C. Johnson, D. Dobberpuhl, R. Roberts and P. Vandeberg, Review. Pulsed amperometric detection of carbohydrates, amines and sulphur spe- cies in ion chromatography - the current state of research, J.
  • Page 80 175_0010 - DECADE Elite user manual - rev 02...
  • Page 81 S/N ratio is obtained. A scanning voltammogram is obtained in the so-called scan mode  of the DECADE Elite: the voltage runs between two pre-set poten- tial values (E1 and E2) and scan speed (in mV/s) and the current is measured.
  • Page 82 175_0010 - DECADE Elite user manual - rev 02 plies the energy level needed to initiate or enhance the electrochemical re- action. Different analytes may have different oxidation or reduction poten- tials, which determines the selectivity of ECD. Fig. 31. Oxidation/reduction reaction of norepinephrine.

  • Page 83: Hydrodynamic And Scanning Voltammogram

    Chapter 5 Detection and Parameters Hydrodynamic and scanning voltammogram Hydrodynamic voltammogram A hydrodynamic voltammogram is constructed when the pure analyte is not available and separation over an analytical column is required. Further- more, under real chromatographic conditions reliable information about the S/N ratio is obtained.
  • Page 84 175_0010 - DECADE Elite user manual - rev 02 Scanning voltammogram An alternative for the chromatographic construction of an I/E relationship is the application of scanning voltammetry. In a scanning voltammetry experi- ment the working electrode potential is ramped up and down between two preset potentials (E1 and E2) and the current is measured while the ana- lyte is continuously flushed through the flow cell.
  • Page 85 Chapter 5 Detection and Parameters As can be seen in both Fig. 32 and Fig. 34, when the working potential is increased the electrochemical reaction is enhanced hence the signal in- creases. At a certain potential the I/E curve flattens. All analyte molecules that reach the working electrode are converted at such a high rate that the analyte supply becomes the limiting factor.
  • Page 86 175_0010 - DECADE Elite user manual - rev 02 Optimization using a voltammogram Sometimes, when interfering peaks appear in the chromatogram, it is pos- sible to optimize the method with regard to selectivity. If the interfering compound has a higher oxidation potential, a working potential is chosen that gives the best selectivity, i.e.
  • Page 87 Also the background signal is sensitive towards fluctuations in the flow rate. Therefore, it is important to use a pulse-free solvent deliv- ery system like in the Antec ALEXYS LC-EC analyzer.
  • Page 88 175_0010 - DECADE Elite user manual - rev 02 Construction of a hydrodynamic voltammogram Before a hydrodynamic voltammogram can be obtained, the chromato- graphic conditions should be optimized. Then the following steps are taken: 1. A solution of the analyte at a concentration between 1 - 100 µmol/l, is prepared in mobile phase.
  • Page 89 Detection and Parameters Construction of a scanning voltammogram A scanning voltammogram can be recorded using the DECADE Elite scan mode. The scan mode is programmed in the ‘SCAN SETUP’ screen of the DECADE Elite. Depending on the data acquisition software that is used and the experimental set-up, a full, half or continuous scan cycle can be chosen.
  • Page 90 In the figure below a scan- ning voltammetry set-up is shown. Fig. 40. DECADE Elite scanning voltammetry set-up with a syringe pump. The Antec dual syringe infusion pump (pn 188.0035) which can be ob- tained as accessory has as an advantage that it can be controlled in Elite Dialogue software as well.
  • Page 91 Chapter 5 Detection and Parameters In the example below a half scan is shown at a flow rate of 10 µL/min of a 20 µM Serotonin (5-HT) standard in mobile phase. Fig. 42. Scan (cycle: half) of a 20 µM Serotonin in mobile phase at a glassy carbon working electrode.
  • Page 92 175_0010 - DECADE Elite user manual - rev 02 ‘detector’ tab in Dialogue. Typical scan settings to start with: E1 0 mV, E2 1000 mV, scan speed 10 mV/s, range 5 µA/V. Optimize the settings if required for your specific compounds.

  • Page 93: Specifications Decade Elite

    2.5 AT / 250V, 5x20 mm, IEC 60127-2 For safety reasons, any other internal fuse or circuit breaker is not operator accessible, and should be replaced only by Antec authorized personnel. Only use manufacturer-supplied fuses. For optimum analytical performance it is recommended that the ambient temperature of the laboratory be between 20-25 °C and be held...
  • Page 94 175_0010 - DECADE Elite user manual - rev 02 General Operating modes DC, PULSE SCAN (Lite: DC mode only) Other mode CONFIG, DIAG and SERVICE Sensors Up to 3 flow cells (Lite: single cell only) Autozero triggered by keyboard, rear panel TTL, or re- mote PC control (LAN) Max.
  • Page 95 CHAPTER 10 Specifications DECADE Elite PULSE mode Range 10 nA - 200 µA in 1, 2, 5 increments Filter (ADF) 0.5 - 0.001 Hz in 1, 2, 5 increments OFF: for unprocessed data Potential (Ec) -2.50 V to + 2.50 V with 10 mV increments...
  • Page 96 175_0010 - DECADE Elite user manual - rev 02...

  • Page 97: Rear Panel I/O

    C H A P T E R Rear panel I/O In this chapter all rear panel functionality is described. The DECADE Elite has besides the mains inlet in total 5 connectors on the rear panel for com- munication, data output and I/O. A photo of the rear panel connectors is shown below for reference.

  • Page 98: Usb B Connector

    175_0010 - DECADE Elite user manual - rev 02 USB B connector USB type B connector for serial instrument control over USB, for service use only: Based on USB-to-serial UART interface using the FT232R chip  from FTDI (Future Technology Devices International Ltd).
  • Page 99 CHAPTER 11 Rear panel I/O Automatic detection of electrically actuated Vici valve, valve  control in: STAT screen and RS232 command ID 30 (0=load, 1=inject). Manual valve status (load/inj) read-out via pin 5 and 6 (contact  closure).  Inject Marker (pin 9) TTL output. Default: high 3.3V (load), on inject event: low (0 V) for 2000 ms.
  • Page 100 175_0010 - DECADE Elite user manual - rev 02 For a manual valve the status (LOAD/INJ) read-out is established by con- necting the LOAD/INJ sensor wires/leads of a manual valve to pin 5 and 6 (contact closure).
  • Page 101 In stand-alone mode the valve position can be controlled via the F5 func- tion button in the STAT screen. For example see the screen dumps of the STAT screen for a DECADE Elite SCC (top) and TCC detector. INJ=L rep- resents the LOAD position (position A on the actuator control module) and INJ=I represents the INJECT position (B on the actuator control module).

  • Page 102: Analog Data Connector

    I/E converter, or the processed data signal by the CPU of the DECADE Elite. The type of output can be selected from the CONFIG screen by setting the parameter Vout source to either DAC or I/E.
  • Page 103 100M, 10M, 1M, 100K or 1K in the I/E converter circuit. DAC output The DAC output is the processed signal by the DECADE Elite’s CPU and is identical to that of the digital cell current signal obtain via data-acquisi- tion over LAN using the Elite Dialogue or the Clarity Chromatography soft- ware.

  • Page 104: Digital I/O Connector

    175_0010 - DECADE Elite user manual - rev 02 Table VI. DECADE Elite I/E converter resistors Current Ranges I/E Resistor (Ohm) 10pA, 20pA, 50pA, 100pA, 200pA, 500pA and 1nA 100M 2nA, 5nA 10nA, 20nA, 50nA 100nA, 200nA, 500nA, 1µA, 2µA 100K 5µA, 10µA, 20µA, 50µA, 100µA, 200µA...
  • Page 105 0.25 A. The relays can be controlled in the Elite Dialogue software and Clarity Chromatography software. The DECADE Elite has 4 free programmable TTL outputs AUX1 – AUX4 (pin 7 – 10). These contacts are default ‘high’ 3.3V (inactive), when active the status is ‘low’...
  • Page 106 1 is ‘out of range’ the status of the overload output will change to ‘low’ 0V. For all other cells present in the DECADE Elite (in case of a DCC or TCC version of the instrument) an out of range situation will not trigger a re- sponse on pin 11.
  • Page 107 ‘Out of range’ the overload input pin 11 will become active. Cell on, Cell off The DECADE Elite has 3 TTL inputs to switch on cells (pin 12 – 14) and also 3 inputs to switch off cells (pin 15 -17) AUX1 – AUX4 (pin 7 – 10).
  • Page 108 175_0010 - DECADE Elite user manual - rev 02 Table VIII. DIGITAL I/O connector layout. Type I/O Function Configurable Description (default) 1,2,3 Relay 1 Relay 1 Contact between 3 (com- mon) and 1 (default), acti- vated by time file Outp 0100...

  • Page 109: Troubleshooting

    Instrument errors Incidental fault conditions may occur in any instrument. The DECADE Elite will generate an error message containing an error number with a short de- scription for several hardware fault conditions.
  • Page 110 Divergent mains voltage Check line voltage Make sure the DECADE Elite is connected to a grounded power source with a line voltage which is within the specified ratings. If the DECADE Elite does not respond, a fuse in the mains inlet may be blown.

  • Page 111: Analytical Troubleshooting

    The first step is to determine whether the problem is caused by the DECADE Elite electrochemical detector or the rest of the (U)HPLC system. For that purpose two basic checks should...

  • Page 112: Dummy Cell Test

    175_0010 - DECADE Elite user manual - rev 02 Dummy cell test External dummy cell An external dummy flow cell (pn 250.0040) is shipped with every DECADE Elite instrument for troubleshooting purposes and maintenance checks. A successful dummy cell test confirms that the controller, including the cell cable, functions properly.

  • Page 113: Stop Flow Test

    Internal dummy cell The DECADE Elite also has the option to run a so-called internal dummy cell test. This exclusively checks the performance of the electronic circuit boards (amplifier circuitry) only, so it excludes the cell cables and the ex- ternal dummy flow cell.
  • Page 114 175_0010 - DECADE Elite user manual - rev 02 Switch off the (U)HPLC pump.   Disconnect the tubing connection from the column outlet (see figure below).  Disconnect the outlet tubing from the flow cell. Connect the other end of the tubing (of the tubing connected to the ...
  • Page 115 CHAPTER 12 Troubleshooting Noise: If a significant drop of the noise only is observed it could be signa- ture of for example pump problem (check valves, air in pump head, com- pressibility issues or leaking seals). In case no significant drop in noise or cell current is observed service or replace the cell.
  • Page 116 175_0010 - DECADE Elite user manual - rev 02 Please bear in mind that analytical problems may also be caused by exter- Influences like temperature, unstable samples. Make sure that the applica- tion was running trouble-free before and that no changes have been made to the system.
  • Page 117 CHAPTER 12 Troubleshooting Noisy baseline Possible cause Remedy Salt bridge in REF not satu- Refill with saturated KCl, add wetted KCl rated crystals Air bubble in REF or in cell Remove air bubble, continuously degas the mobile phase Slow temperature fluctua- Isolate detector cell, set oven temperature tions Fouled WE...
  • Page 118 175_0010 - DECADE Elite user manual - rev 02...

  • Page 119: Detector Accessories

    For a Vici Valco electrically-actuated 2-position valve, with an E2CA, EHCA actuator a serial cable is available for control via the DECADE Elite detector: pn 250.0190 Serial valve cable, Valco, 2m. For these and other DECADE Elite parts or flow cells contact your local...

  • Page 120: Index

    175_0010 - DECADE Elite user manual - rev 02 Index...
  • Page 121 Index ADF, 67 Amplitude response, 71 auxiliary electrode, 57 Buffer pH, 31 buttons DECADE II keyboard, 41 cleaning of detector, 38 compensation, 62 cut off frequency, 72 degassing mobile phase, 34 digital filter, 70 DSP, 71 dual flow cell control, 59 dual flow cell navigation, 61 dummy cell external, 114...
  • Page 122 175_0010 - DECADE Elite user manual - rev 02 frequency, 80 pulse mode, 80 passivation with nitric acid, 34 polarity, 63 potential optimisation, 83 pulse mode characteristics, 78 literature references, 81 optimisation, 79 output frequency, 80 potential settings, 79 working electrode, 80...

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