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Eicom ECD-700 User Manual

Electrochemical detector
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User's ManUal
AC16-0816
Electrochemical Detector
ECD-700
www.eicomusa.com

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Summary of Contents for Eicom ECD-700

  • Page 1 User’s ManUal AC16-0816 Electrochemical Detector ECD-700 www.eicomusa.com...
  • Page 3 ELECTROCHEMICAL DETECTOR ECD-700 USER’S MANUAL (For 1-channel amperometric model) ©2016 Eicom Corporation. All rights reserved.

  • Page 4: Table Of Contents

    Table of Contents SAFETY ................................ 1 1. UnpACking ..............................2 2. nECESSARY COnDiTiOnS ......................... 3 2.1. place for installation ........................3 2.2. power Sources ..........................3 2.3. grounding ............................3 2.4. Recommended Conditions for HpLC pumps................3 3. SYSTEM COnFigURATiOn ......................... 4 3.1.
  • Page 5 6. MAinTEnAnCE ............................27 6.1. Working Electrode ........................27 6.2. Reference Electrode ........................27 6.3. gasket ............................27 6.4. Maintenance of Electrodes ......................28 7. STORAgE ..............................32 8. REpRESEnTATivE ExAMpLES OF ELECTROCHEMiCALLY DETECTAbLE SUbSTAnCES ....33 9. TROUbLESHOOTing ..........................36 10. ORDERing inFORMATiOn ........................37 AppEnDix ...............................

  • Page 6: Safety

    safety Read this manual carefully and in full. All safety and operating instructions should be read before installation and operation. Retain this manual. The safety and operating instructions should be retained for future reference. This instrument should only be used in the laboratory or similar indoor environment, for analytical purposes. Operation of this instrument should only be performed by personnel trained in laboratory work, and who are aware of the possible dangers involved.

  • Page 7: Unpacking

    Check the packaging to ensure there was no damage during transportation. After unpacking, please check the appearance of the instruments. All the parts in the package must be checked off against the list below. If damages or extraordinary conditions are observed on them, please contact your local distributor or EICOM. List of Parts and Accessories...

  • Page 8: Necessary Conditions

    2. NECESSARY CoNdItIoNS 2.1. Place for Installation ECD-700 is designed only for indoor use. Do not expose to direct sunlight, high humidity or dust. Place on flat and stable surface in a room with minimal temperature variation. 2.2. Power Sources ECD-700 should only be operated by a 100V-240V AC 50/60Hz power source.

  • Page 9: System Configuration

    3. SYStEM CoNFIGURAtIoN Overview of ECD-700 is illustrated below. Shield Box Circuit Board Slot Control Panel Electrolysis Cell Fig. 1 System Overview Outlet (to waste bottle) Reference Electrode Working Electrode and Gasket Inlet (from separation column) Fig. 2 Electrolysis Cell Email: info@eicomeurope.com...

  • Page 10: Control Panel

    3.1. Control Panel Display A.ZERO A.ZERO ON/OFF CHANNEL ECD 1&2 ECD 3 CLEAR Control Keys + / － SELECT E S C L O G ENTER Fig. 3 Control Panel Email: info@eicomusa.com Phone: (888) 680-7775...
  • Page 11 Name Function Turning ON/OFF ECD. ECD ON/OFF To turn OFF ECD, press more than 1 sec. (This protects ON/OFF from undesired shutoff of ECD by mistake). Select ECD channels. ECD channel (For additional channels. Not in use on standard model) CHANNEL Auto zero Offset ECD output signal of channel 1&2 to 0 V.

  • Page 12: Left Side Panel

    (>0.3 sec) is available. SIG. IN and SIG. OUT When ECD-700 receives a signal on SIG. IN terminal, delayed signals are automatically sent out from SIG. OUT terminals. CONT. is for contact closure input and O/C is for Open/Close signal input.
  • Page 13 Fig. 6 Connection of ECD-700 with External Equipment. Email: info@eicomeurope.com Phone: +(353) 1 902-2700...

  • Page 14: Rear Panel

    3.4. Rear Panel Power Socket Fuse Grounding Terminal Fig. 7 Rear Panel Email: info@eicomusa.com Phone: (888) 680-7775...

  • Page 15: Electrolysis Cell System

    The electrolysis cell is set in the shielding box to avoid rapid temperature changes and electric noises. Therefore, the lid of the shield should be firmly closed during analysis. When the EICOM column oven ATC-700 is used with the ECD-700, remove the round shaped upper/bottom cover of shield box and set a duct of ATC-700 into the upper/bottom opening of the ECD-700.
  • Page 16 Close the cell block, and then insert the stopper pin into the cell Stopper Pin Cell Block Push the handle up to lock the cell. The tip of reference electrode was sealed by a small glass cuvette filled with 0.1 mol/L LiCl and Reference Electrode acetic acid solution before shipping.
  • Page 17 Reference Electrode Insert the reference electrode into the setscrew and the orange colored o-ring. A setscrew is O-ring (P4) initially mounted on the cell block. DO NOT use Setscrew the white colored silicone o-ring initially used for sealing of electrode. Guide Rod Insert the electrode parallel with the notch in the guide rod into the side opening and fix it by the...
  • Page 18 Fix cell onto the mount and slide the cell into the shield box. Cell Mount Pass the cell inlet and outlet (waste) tubes through access ports. Connect red, black and white wires to R, W1 and C sockets of ECD 1&2 located on the upper left of the shield box, respectively.

  • Page 19: Construction Of Whole Hplc System

    3.6. Construction of Whole HPLC System Basic system constructions are illustrated in Fig. 8 to 10. For high sensitivity measurements, EICOM 700 series HPLC equipment is best suited as it provides inert flow lines, high degassing capacity, computer controlled pulse quenching function and accurate temperature control.
  • Page 20 Waste ECD-700 Precolumn (Guard Column) Separation Column Column Oven (ATC-700) Mobile Phase HPLC Pump and Degassing Unit (EP-700) Autosampler “INSIGHT” (AS-700) Fig. 9 Automated Injection System. Email: info@eicomusa.com Phone: (888) 680-7775...
  • Page 21 Waste ECD-700 Autoinjector (EAS-20) Separation Column Column Oven (ATC-700) Mobile Phase HPLC Pump and Degassing Unit (EP-700) Fig. 10 Microdialysis Automated Injection System. Email: info@eicomeurope.com Phone: +(353) 1 902-2700...

  • Page 22: Principle Of Detection And Specifications

    4. PRINCIPLE oF dEtECtIoN ANd SPECIFICAtIoNS 4.1. Principle The basic principle of electrochemical detection is based on the measurement of the electric current derived from the electrochemical reaction of analytes taking place on the surface of electrodes (Scheme 1). +550 mV vs.

  • Page 23: Applied Potential

    against the working electrode. Desired potential is applied on the counter electrode versus the working electrode. However, due to formation of electric double layer and potential drop (IR-drop) caused by electric resistance of the mobile phase, actual potential between the working electrode and the mobile phase may differ from the desired potential.

  • Page 24: Measurement With Electrolytic Oxidation Current

    4.2.4 Stabilization Time ECD-700 poses high background current just after it is started up or applied voltage is altered, and it gradually reduces to a steady state. Under normal conditions, 30 to 60 minutes may be required to stabilize the background current.

  • Page 25: Selection Of Working Electrodes And Their Features

    4.2.5. Selection of Working Electrodes and Their Features Working Electrode Model Features EICOM standard electrode Best suited for sensitive monoamine analysis High S/N ratio, Economical, Graphite WE-3G Maximum concentration of organic solvent is limited; Methanol: <30%, Acetonitrille: <3% Maximum voltage; <+1,500 mV...

  • Page 26: Specifications

    4.3. Specifications Standard Model Principle Amperometric DC detection Flow Cell 1-channel thin layer type amperometric Circuit Board 1 flow cell 2-channel amperometric detection capable Empty Slot Applied Potential (Ch.1) 0 ~ ± 2,000 mV, 1 mV step Applied Potential (Ch.2) Applied Potential (Ch.1) Auto Zero Working Range ±...

  • Page 27: Operation

    If the pump is new or has been left non-operational for a long time, cleaning the pump lines is required. EICOM HPLC pump EP-700 does not require special pretreatment as it has inert flow lines and is thoroughly cleaned before shipping. After nitric acid cleaning, deliver 1 L of 0.1 mol/L phosphate buffer (pH 3.5) containing 100 mg/L EDTA-2Na, and then replace it with the mobile phase.

  • Page 28: Waste Tube

    Time constant: 1.5 sec 1) Switch on ECD-700. Initially, start-up diagnosis screen appears. After self diagnosis is done, normal screen which accepts parameter changes appears. If you do not need to change parameters from previous ones, you can skip to item 2) as ECD-700 stores previous parameters.
  • Page 29 Press 4 , 5 , 0 keys to set desired applied potential  Press SET / ENTER key once to enter the parameter. The cursor moves to the next line. Press +/-/ SELECT key twice to select 3.0 sec for time constant. 1.0 sec, 1.5 sec and 3.0 sec are scalable for this parameter.

  • Page 30: Log

    5) After the baseline is stabilized, start the analysis. 5.3. ECD-700 can save a log of the replacement of electrodes. Please note that these logs are NOT automatically updated. If you need to keep logs, please renew them manually. 5.3.1.
  • Page 31 If you are sure you need to delete current log, press +/- / SELECT to select ‘YES’ and press SET/ENTER . After deletion of current log, renew a date.  Press number keys (0 -9) to set date (YYYY/MM/DD) and press SET/ENTER key once. Cursor moves to the next line.

  • Page 32: Maintenance

    In such case, baseline noise becomes higher. The liquid junction (white porous ceramic tip) of the reference electrode should NOT be dried. If ECD-700 is not used for more than 1 month, dismount the reference electrode from the cell and immerse the tip in 1 mol/L LiCl solution.

  • Page 33: Maintenance Of Electrodes

    6.4. Maintenance of Electrodes Disconnect red, black and white wires from shield box terminals and pull out the electrolysis cell. Then, unscrew the outlet screw. Aspirate liquid in the cell by a disposable syringe with a needle from the top opening. Without this step, liquid remaining in the cell will cause leakage issues when it is opened.
  • Page 34 Pull out the cell block stopper pin and open the cell Stopper Pin block forward. Cell Block Setting Plate Working Electrode Lift and dismount a setting plate, a working electrode and a gasket. Please note the correct Gasket order of parts. Each part should be reassembled in correct order as illustrated in the figure.
  • Page 35 Check the cutting edge of the gasket. If the edge of it has gotten wrinkled or cracked, please replace it with a new one. Cutting Edge of Gasket Hole Reference Electrode To dismount the reference electrode, unscrew the white setscrew located on the left side of the cell block and pull out the reference electrode.
  • Page 36 Guide Rod To mount the reference electrode, insert the electrode parallel with guide rod rabbet into side opening and fix it by the setscrew. Email: info@eicomusa.com Phone: (888) 680-7775...

  • Page 37: Storage

    7. StoRAGE ECD-700 can be stored with mobile phase in it if storage duration is shorter than 1 month. Avoid dehydration of the flow lines of the electrolysis cell when it is stored with mobile phase as precipitation of salts in the mobile phase will clog the flow lines.

  • Page 38: Representative Examples Of Electrochemically Detectable Substances

    8. REPRESENtAtIVE EXAMPLES oF ELECtRoCHEMICALLY dEtECtABLE SUBStANCES Phenols Tyrosine, Tyramine, Thyroxine, Thyronine, etc. +800 mV - +900 mV (vs. Ag/AgCl) Catechols Epinephrine, Norepinephrine, Dopamine, L-DOPA etc. +400 mV - +700 mV (vs. Ag/AgCl) Methoxyphenols Homovanilic acid, Methanephrine, Normethanephrine, Vanilic acid etc. +800 mV - +900 mV (vs.
  • Page 39 Hydroxycoumarins Scopoletin etc. +800 mV - +900 mV (vs. Ag/AgCl) Tocopherols α-, β-, γ-, δ- Tocopherols +700 mV (vs. Ag/AgCl) N CH Morphine Morphine +800 mV (vs. Ag/AgCl) Phenothiazines Chlorpromazine, Promethazine, Perphenazine etc. +900 mV (vs. Ag/AgCl) Purines Uric acid, Xanthine, Guanine, Theophylline etc. +800 mV - +1100 mV (vs.
  • Page 40 Thiols RS H Cysteine, Glutathione, Penicillamine etc. +600 mV - +800 mV (vs. Ag/AgCl) Acetylcholine Detectable after conversion into H2O2 by a post-column enzyme reactor. +450 mV (vs. Ag/AgCl) α-amino acids COOH Detectable after reaction with o-phtalaldehyde (OPA). +500 mV - +700 mV (vs. Ag/AgCl) Anions SCN-, S2O32-, SO3-, NO2- etc.

  • Page 41: Troubleshooting

    Baseline drift them well. Use inert (metal free) pumps. Decreased sensitivity Ground ECD-700 and other HPLC Electrostatic noise on HPLC systems equipment including data processors and or columns. columns each other, see 3-3. Sensitivity range setting is wrong Reset the range.

  • Page 42: Ordering Information

    10. oRdERING INFoRMAtIoN Parts Product Type Catalog Code Graphite Working Electrode WE-3G 100010 Pure Graphite Working Electrode WE-PG 100040 Glassy Carbon Working Electrode WE-GC 100020 Platinum Working Electrode WE-PT 100030 Gold Working Electrode WE-AU 100050 Silver Working Electrode WE-AG 100060 Reference Electrode RE-500 100500...

  • Page 43: Appendix

    APPENdIX CPU I/O Control Email: info@eicomeurope.com Phone: +(353) 1 902-2700...
  • Page 44 United States Europe 7098 Miratech Drive, Suite 100, Hilton House Ardee Rd, Ground Floor, San Diego, California 92121 Rathimines Dublin 6, Ireland info@eicomusa.com E. info@eicomeurope.com 888.680.7775 +(353) 1 902-2700 858.560.8040 +(353) 1 443-0784 www.eicomusa.com www.eicomeurope.com...

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