Related Manuals for Antec Scientific DECADE II SDC 174
Summary of Contents for Antec Scientific DECADE II SDC 174
- Page 1 Antec Scientific Industrieweg 12 2382 NV Zoeterwoude The Netherlands DECADE II SDC Electrochemical Detector User manual 171.0011, Edition 12, 2015 T +31 71 5813333 | info@AntecScientific.com | https://AntecScientific.com...
- Page 2 Copyright ©2015, Antec, The Netherlands. Contents of this publication may not be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from the copyright of the owner. The information contained in this document is subject to change without notice. ROXY, ALEXYS, DECADE, DECADE II, INTRO, Flexcell, ReactorCell, SenCell, VT-03, µ-PrepCell, SynthesisCell, ISAAC, HyREF are trademarks of Antec.
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Page 3: Declaration Of Conformity
Chapter 1 DECADE II SDC Declaration of conformity We Antec Leyden B.V., Zoeterwoude, The Netherlands, declare that the product DECADE II SDC ™ Electrochemical Detector type 174 to which this declaration relates, is in conformity with the following directives: Safety (2006/42/EC) Safety requirements for laboratory equipment IEC61010-1:2001 2 (Class I, Installation cat. -
Page 4: Intended Use
DECADE II SDC user manual, ed. 3. Intended use For research purposes only. While clinical applications may be shown, this instrument is not tested by the manufacturer to comply with the In Vitro Diagnostics Directive. 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 requirements. -
Page 5: Symbols
Chapter 1 DECADE II SDC 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) -
Page 6: Safety Practices
DECADE II SDC user manual, ed. 3. Safety practices The following safety practices are intended to insure safe operation of the equipment. Electrical hazards The removal of protective panels on the instrument can result in exposure to potentially dangerous voltages. Therefore, disconnect the instrument from all power sources before disassembly. -
Page 7: Spare Parts And Service Availability
Chapter 1 DECADE II SDC socket. The power source should exhibit minimal power transients and fluctuations. Replace faulty or frayed power cords. Place the detector on a flat and smooth surface. Do not block the fan located at the bottom of the detector. Blocking the fan will impair the cooling capability of the power supply. - Page 8 DECADE II SDC user manual, ed. 3.
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Page 9: Table Of Contents
Chapter 1 DECADE II SDC Table of contents Declaration of conformity 3 Intended use 4 WEEE directive 4 ROHS directive 4 Symbols 5 Safety practices 6 Spare parts and service availability 7 DECADE II SDC 11 Installation guide 13 Unpacking 13 Installation 13 Maintenance 17 ALEXYS... - Page 10 DECADE II SDC user manual, ed. 3. Optimisation of working potential 35 Introduction 35 Electrochemical reactions 35 Hydrodynamic voltammogram 36 Optimisation using a voltammogram 37 Construction of a hydrodynamic voltammogram 39 Specifications DECADE II SDC 41 General specifications 41 Physical specifications 42 Error messages 43 Rear panel 44 Connectors A, B and C 44...
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Page 11: Decade Ii Sdc
Chapter 1 DECADE II SDC C H A P T E R DECADE II SDC Congratulations on your purchase of the DECADE II SDC. This detector enables you to perform all applications using electrochemical detection in the DC mode. The DECADE II SDC includes a highly stable Faraday-shielded oven compartment accommodating column and flow cell. - Page 12 DECADE II SDC user manual, ed. 3.
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Page 13: Installation Guide
CHAPTER 2 Installation guide C H A P T E R Installation guide Unpacking Inspect the transport box for possible damage as it arrives. Immediately inform the transport company in case of damage, otherwise she may not accept any responsibility. Keep the transport box as it is designed for optimum protection during transport and it may be needed again. - Page 14 DECADE II SDC user manual, ed. 3. Table I. Environmental conditions Parameter Requirement -40 – 50 C (-104 – 122 Storage temperature 0 – 90%, non-condensing Storage humidity 4 – 40 C (39 – 104 Operating temperature 20 – 80%, non-condensing Operating humidity Place the detector on a flat and smooth surface.
- Page 15 CHAPTER 2 Installation guide up to 10 mL/min. Please carefully follow the next steps for a successful installation and start-up. 1. The installation of the flow cell and column is shown in Fig. 3. 2. If a manual injector is applied with position sensor, the sensor cable must be connected to ‘C’...
- Page 16 DECADE II SDC user manual, ed. 3. 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 chloride (KCl or NaCl) ions. 6.
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Page 17: Maintenance
CHAPTER 2 Installation guide 12. Set the cell potential (see page 35 for optimisation of the potential), switch ON the flow cell (see page 17) and allow the system to stabilise for approximately 30 min. A ‘good’ stabilisation curve shows a mono-exponential decline without jumps and/or spikes. -
Page 18: Alexys ® Decade Ii Sdc Driver
DECADE II SDC user manual, ed. 3. ® ALEXYS DECADE II SDC driver Full control and data acquisition is supported in the ALEXYS data system software. Important difference with stand-alone operation is that timed events are not executed from time files, but from the events page in the ALEXYS software. -
Page 19: Decade Ii Dialogue For Sdc
CHAPTER 2 Installation guide DECADE II Dialogue for SDC DECADE II Dialogue for Windows is a multi-functional program to control the DECADE II electrochemical detector. DECADE II Dialogue is a tool for: • controlling all operational parameters of DECADE II •... - Page 20 DECADE II SDC user manual, ed. 3. Fig. 6. DECADE II Dialogue for operational control of the DECADE II SDC electrochemical detector.
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Page 21: Detection And Parameters
CHAPTER 4 Detection and parameters C H A P T E R Detection and parameters Introduction One of the characteristics of electrochemical detection is its tremendous dynamic range. In amperometric detection peak heights may vary from micro-amperes down to the pico-ampere range. The DECADE II SDC covers such a wide range from 200 µA down to 10 pA full scale, without being limited by electronic noise. -
Page 22: Parameters
DECADE II SDC user manual, ed. 3. Parameters Operational parameters are controlled using PC software. Range A number of ranges can be selected; the maximum current that can be compensated for using auto zero and offset differs. The high sensitivity ranges (10 pA - 5 nA) have the best noise specifications. -
Page 23: Offset
CHAPTER 4 Detection and parameters Offset A maximum offset of +50% and - 50% in 5% steps can be set. For example, 20% is a 200 mV offset when the maximum output is 1.0 Volt (2 V at max. 10.0 V). Polarity The polarity of the output can be inversed. - Page 24 DECADE II SDC user manual, ed. 3.
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Page 25: Noise Suppression: Adf
Noise suppression: ADF™ CHAPTER 5 C H A P T E R Noise suppression: ADF™ Introduction Besides for its tremendous linear dynamic range and selectivity, electrochemical detection is well-known for its very low limits of detection. To further improve these detection limits the Antec Leyden engineers have developed ADF (Advanced Digital Filter) and the DECADE II has been equipped with it as a standard. -
Page 26: Frequency Of Signal And Noise
DECADE II SDC user manual, ed. 3. 400000 300000 200000 100000 -100000 -200000 -300000 -400000 Fig. 9. Example of a signal with regular evenly spaced alterations: a sine. 400000 300000 200000 100000 -100000 t (min) -200000 -300000 4.15 4.56 -400000 Fig. - Page 27 Noise suppression: ADF™ CHAPTER 5 This is further illustrated by an overlay of the same chromatographic peak with a sine of 0.07 Hz (Fig. 12). 540000 440000 340000 240000 140000 40000 Fig. 12. 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.
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Page 28: Low Pass Noise Filters
DECADE II SDC user manual, ed. 3. sine f = 10 Hz sine f = 0.4 Hz t (s) Fig. 14. Typical random noise in chromatography (lower trace). Both frequencies (0.4 and 10 Hz) can be recognised amongst others. Looking closely to the lower noise trace both frequencies (and others) can be recognised. -
Page 29: Amplitude Response Plot
Noise suppression: ADF™ CHAPTER 5 Each input data point has the same weighting factor of 1/5. In more advanced digital signal processing a more complicated equation is used to calculate the output data point y[n]: In contrast to the previous equation, each data point has a different weighting factor a. - Page 30 DECADE II SDC user manual, ed. 3. This cut off frequency is where the output signal amplitude is 70% of the input signal, also known as 3 dB point. Freq uency (Hz) Fig. 16. An amplitude response plot of a low pass filter with a cut-off frequency of 1 Hz.
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Page 31: Applying Adf In Chromatography
Noise suppression: ADF™ CHAPTER 5 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 specifically attenuate noise and improve the signal-to-noise (S/N) ratio. No matter how ‘advanced’... - Page 32 DECADE II SDC user manual, ed. 3. of the signal of interest. This is particularly difficult if the frequency of the signal is close to the frequency of the noise. The DECADE II has a number of filter settings to optimise for best possible signal-to-noise ratio.
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Page 33: Events And Time Files
CHAPTER 5 Events and time files C H A P T E R Events and time files Introduction Running an Events table enables a time-based, automated and full parametric control of electrochemical detection (ECD). This is particularly useful when during a run or between runs settings have to be changed such as the sensitivity, auto zero or control of external equipment (i.e. - Page 34 DECADE II SDC user manual, ed. 3. Table III. I/O contacts connector A. Name Function 1,2,3 Relay 1 Contact between 1 (common) and 2 (default) or 3. Activated by time file Outp 0100 4,5,6 Relay 2 Contact between 4 (common) and 5 (default) or 6. Activated by time file Outp 1000 Cell on Trigger to switch on cell...
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Page 35: Optimisation Of Working Potential
CHAPTER 7 Optimisation of working potential C H A P T E R Optimisation of working potential Introduction A current - voltage (I/E) relationship, or voltammogram, characterises an analyte. It gives information on the optimum working potential, which can be used to improve detection sensitivity and selectivity. -
Page 36: Hydrodynamic Voltammogram
DECADE II SDC user manual, ed. 3. electrons are transferred at the WE resulting in an electrical current that is amplified by the controller. Hydrodynamic voltammogram A hydrodynamic voltammogram is constructed when the pure analyte is not available and separation over an analytical column is required. Furthermore, under real chromatographic conditions reliable information about the S/N ratio is obtained In case of metal working electrodes it is also advisable to use a... -
Page 37: Optimisation Using A Voltammogram
CHAPTER 7 Optimisation of working potential With respect to sensitivity, a high working potential is important. 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 less reproducibility. - Page 38 DECADE II SDC user manual, ed. 3. Electrochemical reactions are pH sensitive (Fig. 23). For norepinephrine the I/E curve is shifted to a lower potential at higher pH. When the working potential is high (E ), and the signal is diffusion limited, an increase in pH will result only in a small increase of the peak height.
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Page 39: Construction Of A Hydrodynamic Voltammogram
CHAPTER 7 Optimisation of working potential Fig. 24. Construction of a hydrodynamic voltammogram for norepinephrine. Chromatograms are obtained at cell potentials ranging from 1.0 V (back) to 0.4 V (front), with 100 mV steps. Construction of a hydrodynamic voltammogram Before a hydrodynamic voltammogram can be obtained, the chromatographic conditions should be optimised. - Page 40 DECADE II SDC user manual, ed. 3.
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Page 41: Specifications Decade Ii Sdc
CHAPTER 8 Specifications DECADE II SDC C H A P T E R Specifications DECADE II SDC General specifications Power 100-240 VAC, 50/60 Hz, 260 VA max., auto- sensing Operating mode Potential range between +2.00 and - 2.00 V in 10 mV increments Output between +1 and - 1 V or between +10 and -10 V (20 bit D/A converter) -
Page 42: Physical Specifications
DECADE II SDC user manual, ed. 3. Physical specifications Dimensions 44 (D) x 22 (W) x 44 (H) cm = 17.3” Dimensions (D) x 8.7” (W) x 17.3” (H) Weight 14 kg (32 lbs) without flow cell and column... -
Page 43: Error Messages
CHAPTER 9 Error messages C H A P T E R Error messages Table V. Error messages. Error Message Incompatible boot version Control board error Sensor board x error (x = board number) Firmware program error Record error Incompatible FW version Incompatible FW Control board FW erase failed Sensor board x... -
Page 44: Rear Panel
DECADE II SDC user manual, ed. 3. C H A P T E R Rear panel Connectors A, B and C For detailed information on the I/O contacts see page 34. Fig. 25. DECADE II SDC rear panel. RS232C The RS232 interface provides full parametric control from a PC. Programmable parameters comprise cell potential, range, auto zero, offset, filter and control of DECADE II SDC output contacts for control of external equipment. -
Page 45: Troubleshooting Guide
CHAPTER 11 Troubleshooting guide C H A P T E R Troubleshooting guide No detector response Possible cause Remedy No power Check line voltage setting, plug in power cord Power switch off Turn this switch ON (at the rear panel) Faulty fuse Replace fuse Divergent mains voltage... -
Page 46: Decreased Sensitivity (Low S/N Ratio)
DECADE II SDC user manual, ed. 3. Decreased sensitivity (low S/N ratio) Possible cause Remedy Fouled WE by dirty samples Clean WE, if possible: dilute samples Cell potential too low Optimise potential Contaminated buffer (high Replace buffer, do not recycle the buffer cell Base line oscillations Possible cause... -
Page 47: Dummy Cell
CHAPTER 12 Dummy cell C H A P T E R Dummy cell External dummy cell A successful dummy cell test confirms that the DECADE II SDC, including the cell cable, functions properly. If the result of the noise measurement with the dummy cell is within specs, the DECADE II SDC is excluded in a trouble shooting procedure. -
Page 48: Detector Accessories
DECADE II SDC user manual, ed. 3. C H A P T E R Detector accessories The electrochemical detector is shipped together with a number of parts. The listing in Table below may not be complete, see check list of delivery for complete listing. - Page 49 CHAPTER 14 Detector accessories Index...
- Page 50 DECADE II SDC user manual, ed. 3. ADF, 23 Amplitude response, 27 Auto zero, I/O contact, 31, 32 AUX1, I/O contact, 32 AUX2, I/O contact, 32 Cell off, I/O contact, 32 Cell on (off), I/O contact, 31 cell on, I/O contact, 32 cleaning of detector, 15 Common, I/O contact, 32 compensation, 20...
- Page 51 CHAPTER 14 Detector accessories Overload, I/O contact, 31, 32 passivation with nitric acid, 13 polarity, 21 potential optimisation, 33 range, 20 Relay 1, I/O contact, 32 Relay 2, I/O contact, 32 Reset, I/O contact, 32 RS232C, 42 S/N ratio, 37, 44 safety practices, 5 service, 6 spare parts, 6...
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