Shimadzu ECD-2010 Exceed Instruction Manual
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Shimadzu ECD-2010 Exceed Instruction Manual

Shimadzu ECD-2010 Exceed Instruction Manual

Electron capture detector for gc-2010 plus
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221-79141C
Oct. 2017
Electron Capture Detector For GC-2010 Plus
ECD-2010 Exceed
Instruction Manual
Read this manual thoroughly before you use the product.
Keep this manual for future reference.

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  • Page 1 221-79141C Oct. 2017 Electron Capture Detector For GC-2010 Plus ECD-2010 Exceed Instruction Manual Read this manual thoroughly before you use the product. Keep this manual for future reference.
  • Page 2 This page is intentionally left blank.
  • Page 3 • Since a radioisotope is used as the radiation source, check the laws and regulations before installation. • ECD-2010 Exceed is classified as B64666/IEC60405 and ISO/12/C32211 of ISO2919. • ECD-2010 Exceed must be checked for radiation periodically depending on your local regulation. Important •...
  • Page 4 The following symbols are used in this manual: Notation Description Indicates an action that must not be performed. Indicates information provided to improve product performance. Indicates the location of related reference information. ECD-2010 Exceed...
  • Page 5 Safety Instructions Safety Instructions The ECD-2010 EXceed is a detector for Shimadzu gas chromatograph GC-2010 Plus. The Gas Chromatograph is a gas chromatography system used to perform qualitative and quantitative analysis. To ensure safe product operation, read these important safety instructions carefully before use and follow all DANGER, WARNING and CAUTION instructions given in this section.
  • Page 6 This may result in accidents due to electric shock or short circuits. It may also result in an injury or equipment failure. When repair is necessary, request your Shimadzu representative. Failing to do so may result in an ignition, electric shock, or injury.
  • Page 7 Safety Instructions n Application name plates Stick the name plates at the position shown below: Fig. 1 ECD-2010 Exceed...
  • Page 8 If you find that the GC-2010 Plus has malfunctioned, immediately perform an emergency stop. Also, prior to starting the system again, inspect the instrument thoroughly and, if required, contact your Shimadzu representative. Emergency Shutdown Procedure Turn OFF power to the GC-2010 Plus.
  • Page 9 Shimadzu may not be able to provide identical replacement products. 3. Limitation of Liability: (1) In no event will Shimadzu be liable for any lost revenue, profit or data, or for special, indirect, consequential, incidental or punitive damages, however caused regardless of the theory of liability, arising out of or related to the use of or inability to use the product, even if Shimadzu has been advised of the possibility of such damage.

  • Page 10: Introduction

    Replacement parts for this product will be available for a period of seven (7) years after the product is discontinued. Thereafter, such parts may cease to be available.Note, however, that the availability of parts not manufactured by Shimadzu shall be determined by the relevant manufacturers.

  • Page 11: Table Of Contents

    Setting the detector temperature ....... Setting the temperatures of the column oven and injection port ..........Checking the baseline ........3.10 Setting the current value ........3.11 Setting the range/attenuation ......3.12 Caution during analysis ........3.13 Stopping the system .......... 3.14 ECD-2010 Exceed...
  • Page 12 How to Keep the ECD Cell Clean ....... Cleaning procedure for ECD Cell ......Actions to Be Taken in Case There Is the Doubt of Break ..........Troubleshooting Troubleshooting ..........Error Message ........... Disposal Cautions at Disposal .......... Maintenance Parts Maintenance Parts List ........ECD-2010 Exceed...
  • Page 13 Contents Specifications Specifications of the ECD-2010 Exceed ....Appendix Structure of ECD Cell ......... 10.1 Contact Free Technology ........10.2 Calibration Curve ..........10.3 Conditioning of Equipment ........ 10.4 ECD-2010 Exceed...
  • Page 14 This page is intentionally left blank.

  • Page 15: Outline

    (VFC) to make the two currents equal. The pulse from the VFC is shaped to have appropriate width and height before being sent to the ECD cell, closing a control loop. ECD-2010 Exceed...

  • Page 16: Response Characteristics Of The Detector

    2-dichloroethylene chloroform 6 × 10 carbon tetrachloride 4 × 10 1-bromopropane 1-bromobutane bromocyclopentane 1-bromopropene-2 (allyl bromide) 4 × 10 1, 1-dibromoethane 1.1 × 10 1-iodobutane 9 × 10 benzene 0.06 toluene 2-fluorotoluene 0.55 4-fluorotoluene 0.55 chlorobenzene bromobenzene 1-butanol ECD-2010 Exceed...
  • Page 17 Lindane 11,000,000 Dibromoethane 11,000,000 Fluothane 16,000,000 Carbon Tetrachloride 400,000,000 *1 Phillippe Devaux, Georges Guiochon ; in "Advances in Gas Chromatography 1967", A. Zlatkis, ed. *2 K.P.Dimick, H.Hartmann ; presented at ACS Winter Meeting Cincinnati, Ohio January 13-18, 1963. ECD-2010 Exceed...

  • Page 18: Parts List

    Parts List Parts List This unit consists of the following contents. Confirm these contents. n List of parts for the ECD-2010 Exceed Control unit for the ECD-2010 Exceed (excluding the detector unit) : Part No. 221-77550-42 Part name Part No.

  • Page 19: Basic Operation

    After the detector temperature has reached the set value, wait for 10 minutes or more and then set the injection port and column oven temperatures. After the baseline has been stabilized, press the [Zero Adj.] key (PF menu) on the [MONIT] screen to make the zero adjustment. Start the analysis. ECD-2010 Exceed...

  • Page 20: Gas Used

    The chemical substances found near the detector inlet may cause injury. • Do NOT remove the ECD from the gas chromatograph. (Contact your Shimadzu representative to replace the ECD.) • Do NOT disassemble the ECD to take out any radioisotope.

  • Page 21: Checking The Glass Insert And The Injection Inlet Septum

    O-ring for the glass insert has not yet deteriorated in quality. Fig. 3-1 Glass insert Replace the injection inlet septum, in principle, when the number of injections reaches one hundred (or fifty when using a gas tight syringe). ECD-2010 Exceed...

  • Page 22: Mounting The Column

    Set the column temperature at the analysis temperature plus 20 °C (without exceeding the maximum operating temperature in the isothermal analysis) and then allow the column to stand for approximately 12 hours. While the column is conditioned, the detector shall be sealed. ECD-2010 Exceed...

  • Page 23: Setting The Flow Rate

    Set the flow rate of the carrier gas on the screen that is displayed by pressing the [FLOW] key Also set the column and purge. For the procedural details, refer to "12. Injection Port" in the instruction manual for the GC-2010 Plus (CD-ROM version). Fig. 3-3 ECD-2010 Exceed...

  • Page 24: Setting The Flow Rate Of Detector Gas

    ECD gas. Unless the peak range expands, the sensitivity increases as the flow rate of the ECD gas decreases. Modifying the ECD gas flow rate during a series of analyses changes the detection sensitivity and obstructs correct analysis. Fig. 3-4 ECD-2010 Exceed...

  • Page 25: Starting The System

    The control of the ECD control unit will not be started unless the detector is On. For further details of this procedure, refer to "7. Starting and Stopping GC" in the instruction manual for the GC-2010 Plus (CD-ROM version). Fig. 3-5 ECD-2010 Exceed...

  • Page 26: Setting The Detector Temperature

    1 nA. For the output of digital signals via the GCsolution or other, set the current value only. To change the current value, move the cursor to the current value on the [DET] screen using the UP or DOWN cursor keys. Enter a value and then press the [ENTER] key. ECD-2010 Exceed...

  • Page 27: Setting The Temperatures Of The Column Oven And Injection Port

    Be sure to maintain the detector at a temperature higher by at least 20 °C than the column temperature. Failure to do so may contaminate the ECD cell with the material eluting from the column. Fig. 3-7 ECD-2010 Exceed...

  • Page 28: Checking The Baseline

    The "zero adjust" of the GCsolution is same as the zero adjustment on the GC. But the Chromatopac can not adjust the detector output signal of GC. The zero adjustment should be done on the GC before the zero adjustment on the Chromatopac. ECD-2010 Exceed...

  • Page 29: Setting The Current Value

    To set the current value, move the cursor to the current value line on the [DET] screen using the UP or DOWN cursor key. Enter a value and then press the [ENTER] key to validate the value. Fig. 3-10 ECD-2010 Exceed...

  • Page 30: Setting The Range/Attenuation

    1/100, the range ´10 , 1/1000, and the range ´10 , 1/10000. For the high-sensitivity analysis, therefore, use a small range (´1 or ´10 ). Otherwise, use , ´10 , or ´10 a large range (´10 Fig. 3-11 ECD-2010 Exceed...

  • Page 31: Caution During Analysis

    This difficulty in analysis is attributable to the fact that the ionization efficiency per unit time of nitrogen sent as the makeup gas to the ECD cell decreases. In this case, set the flow rate of the makeup gas to a slightly larger value. ECD-2010 Exceed...

  • Page 32: Stopping The System

    To restart the GC-2010 Plus that has been stopped by the above sequence, do as described in "3.7 Starting the system" P.11. If the GC-2010 Plus is stopped for a long period, close the main valves on the gas cylinders. Fig. 3-12 ECD-2010 Exceed...
  • Page 33 The cell and flow path can be maintained to be clean by sending the makeup gas to the cell even if the ECD is not used. The baseline will become stable earlier when the system is restarted, than in the case where the makeup gas is stopped completely. ECD-2010 Exceed...

  • Page 34: Key Operation

    Setting the detector to "Off" while using the detector controller stops the detector signal output, and setting "On" resumes the output. ： On / Off Selection ： On Default ECD-2010 Exceed...
  • Page 35 You can subtract the base line stored as the background from the COMP. actual base line. By this subtraction, stable base line can be output even if the base line considerably fluctuates. ： Off / Buff1 / Buff2 Selection ： Off Default ECD-2010 Exceed...
  • Page 36 "´2 " to "´1", from "´2 " to "´2 ". In case of the digital signal, the signal is always output with "´1". ： ´1 / ´2 / ´2 / ´2 / ´2 Selection ： ´2 Default ECD-2010 Exceed...

  • Page 37: Pf Menu List

    Det Gas Sets the flow rate of ECD gas (makeup gas + cell purge gas). Next Det Changes over to setup screen for another installed detector. You can change over screen by pressing [DET] key on detector screen. ECD-2010 Exceed...

  • Page 38: Checking The Installation State Setting

    (up/down), input numerical values, and press the [ENTER] key. The relation between the installation position and the number is as follows: (0 = Not installed, 9 = Installed at the position other than those in the figure.) Fig. 4-4 ECD-2010 Exceed...
  • Page 39 Heater port This is the temperature control port of the detector to which flow controller set in the slot is connected. For details, refer to "16.7 Service and maintenance" in the instruction manual for the GC-2010 Plus (CD-ROM version). ECD-2010 Exceed...

  • Page 40: Checking The Detector Setting Of Line Configuration

    (up/down), select the line number, and determine the selection by pressing the [ENTER] key. For details, refer to "8. Setting the Analytical Parameters and File Management" in the instruction manual for the GC-2010 Plus (CD-ROM version). ECD-2010 Exceed...

  • Page 41: Selecting The Detector

    Press the toggle key to select the PF menu. Pressing the [Next Det] can select the other detectors. When changing from FID of DET#1 to ECD of DET#2, the screen is changed as follows: Fig. 4-9 Fig. 4-10 ECD-2010 Exceed...

  • Page 42: Selecting The Detector Gases

    4.3.1 PF menu list PF menu Description Return Returns to the detector setting screen. Program Goes to the detector gas flow rate program screen. On/Off Toggles between turning ON and OFF the control for the flow rates of detector gases. ECD-2010 Exceed...
  • Page 43 • The cell and flow path can be maintained to be clean by sending the makeup gas to the cell even if the ECD-2010 EXceed is not used. The baseline will become stable earlier when the system is restarted, than in the case where the makeup gas is stopped completely.

  • Page 44: Detector On/Off

    4 Key Operation Detector ON/OFF Using the UP and DOWN cursor keys, position the cursor on the desired item. Select ON or OFF by horizontally moving the cursor, and then press the [ENTER] key. Fig. 4-13 ECD-2010 Exceed...

  • Page 45: Setting The Range/Attenuation

    Position the cursor on the indicated item with the UP and DOWN cursor, change the range with the LEFT and RIGHT cursors, and then press the [ENTER] key. Normally, use ´10 ). For the high-sensitivity analysis, use ´1. (´2 Digital signals are output as ´1 regardless of the above setting. Fig. 4-14 ECD-2010 Exceed...

  • Page 46: Setting The Current Value

    However, the noise level simultaneously becomes higher. Move the cursor to the row for the current value using the UP or DOWN cursor key. Enter a value with numeric keys and then press the [ENTER] key. Fig. 4-15 ECD-2010 Exceed...

  • Page 47: Zero Adjustment

    When the displayed line configuration does not include the ECD, press [Chng Line] of the PF menu and change the line. (Press the toggle key when the PF menu does not display [Chng Line].) Fig. 4-16 Fig. 4-17 ECD-2010 Exceed...
  • Page 48 The "zero adjust" of the GCsolution is same as the zero adjustment on the GC. But the Chromatopac can not adjust the detector output signal of GC. The zero adjustment should be done on the GC before the zero adjustment on the Chromatopac. Fig. 4-18 Fig. 4-19 ECD-2010 Exceed...
  • Page 49 4.7 Zero adjustment Key operation No. 2 : Performing manual zero adjustment Pressing [Up] / [Down] of the PF menu changes the baseline level upward/downward. Fig. 4-20 Example: Chromatopac screen Fig. 4-21 ECD-2010 Exceed...
  • Page 50 Pressing the [Zero Free] of the PF menu returns the baseline to the level before zero adjustment is performed. Fig. 4-22 When the level does not move with key operation, it is exceeding upper or lower limit. In such a case, refer to "6.1 Troubleshooting" P.44. ECD-2010 Exceed...

  • Page 51: Checking The Ecd Cell

    ECD current ： 27000 µV lower than 0.3 nA However, even if this limit is exceeded, the analysis can be performed so far as the satisfactory peak can be obtained when the current is set to a smaller value. ECD-2010 Exceed...
  • Page 52 ECD. However, it cannot be changed on the GC-2010 Plus alone. The ECD frequency is in proportion to the detector signal level, and the output frequency of 40 kHz is equivalent to the signal level of 2,500,000 µV. ECD-2010 Exceed...

  • Page 53: How To Keep The Ecd Cell Clean

    350 °C, as possible (for instance 340 °C). "10.4 Conditioning of Equipment" P.56 Conditioning the ECD cell immediately after use is an effective method for extending the operational life of the ECD cell. ECD-2010 Exceed...
  • Page 54 When the column is removed, blank off with the graphite ferrule and the column nut. The make up gas is not flow, while the power is off. Install the blind (G-type nut) to the ECD vent to keep the radiation source clean, when the power is turned off. ECD-2010 Exceed...

  • Page 55: Cleaning Procedure For Ecd Cell

    The ECD cell used for gas chromatography may through long service, be contaminated with samples, column packing or liquidphase, causing sensitivity to drop, abnormal peck shapes or inverted peaks, etc. In such a case contact your Shimadzu representative for cleaning (repair) of the ECD cell in the following procedure: For the mounting and removing the ECD unit, contact your Shimadzu representative.
  • Page 56 • If you have removed the ECD unit, cover the mounting holes with the insulation cut out at the time of installation. Fig. 5-1 Packing example for mailing ECD-2010 Exceed...

  • Page 57: Actions To Be Taken In Case There Is The Doubt Of Break

    Actions to Be Taken in Case There Is the Doubt of Break If there is a doubt of break of the ECD, the measurement with the survey meter must be carried out. If there is any abnormality such as the disuse of the ECD etc. "7 Disposal" P.50 ECD-2010 Exceed...

  • Page 58: Troubleshooting

    Troubleshooting" in the instruction manual for the GC-2010 Plus (CD-ROM version). If a trouble cannot be cleared by the countermeasure given hereafter, or if a troubles other than outlined in this chapter occurs, contact your Shimadzu representative which is nearest to you.
  • Page 59 Temperature of each section is Monitor the temperature of each section on the unstable. monitor screen ([MONIT] key). Contact your Shimadzu representative if the temperature will not stabilize. The flow rate is unstable. Monitor the pressure and flow rate on the monitor screen ([MONIT] key).
  • Page 60 ECD unit to our Company for cleaning. "5 Service/Maintenance" P.37 A component has stuck to the glass Replace the glass insert with an inert one (optional). insert. Replace it with an acid-treated or alkali-treated one for some components. ECD-2010 Exceed...
  • Page 61 • The temperature does not rise. • Column inlet pressure or total flow rate connot be set, or the difference is severe. • Ghost peak. • Abnormal peak shape. • Reproducibility of retention time is low. • Reproducibility of peak area is low. ECD-2010 Exceed...

  • Page 62: Error Message

    When the message persists even after the calibration, the valve inside the APC may be broken. Turn OFF the power to the system and contact your Shimadzu representative. DetAPCx ECDG is out of ctrl. Make sure that the supply pressure of the detector gas is sufficient to the set flow rate.
  • Page 63 6.2 Error Message n Error due to incorrect input ECDGx calc. prss out of rng. The pressure value calculated from the set flow rate exceeds the available set range. Change the detector gas flow rate. ECD-2010 Exceed...

  • Page 64: Cautions At Disposal

    Also, in the case of disposing the gas chromatograph equipped with the ECD, be sure to remove the ECD and take the measures mentioned above. When removing the ECD from the gas chromatograph, contact your Shimadzu representative. Keep the original packing container for future transportation of the ECD unit.

  • Page 65: Maintenance Parts List

    Column GaskeT Aluminum (500 201-35183-84 Packing for the piping joint pcs.) For removing contamination in Molecular sieve filter 221-34121-94 carrier gas and makeup gas Trap (SPLIT) 221-42559-92 Split flow line trap Trap (PURGE) 221-42559-92 Septum parge flow line trap ECD-2010 Exceed...

  • Page 66: Specifications Of The Ecd-2010 Exceed

    Specifications Specifications of the ECD-2010 Exceed ： Type Frequency-controlling, constant current type ： Radiation source Ni 370 MBq ： Cell Coaxial type electrode with purging line ： Cell current 0.00 to 3.50 nA ： (with g-BHC) Dynamic Range ： Detection limit 4 fg/s ：...

  • Page 67: Appendix

    Appendix 10.1 Structure of ECD Cell Fig. 10-1 Structure of the ECD unit ECD-2010 Exceed...

  • Page 68: Contact Free Technology

    10 Appendix 10.2 Contact Free Technology The ECD-2010 Exceed employs a technology which allows sample components contained in carrier gas to barely contact the surfaces of the collector electrode and the radiation source. This is called "Contact Free Technology". Contact Free Technology prevents contamination of the ECD cell.

  • Page 69: Calibration Curve

    Even if the calibration is not linear, if it is within the dynamic range, quantitative analysis is possible using a two-point calibration curve method. Note, however, that quantitative analysis is not possible beyond the dynamic range. Fig. 10-3 ECD-2010 Exceed...

  • Page 70: Conditioning Of Equipment

    Setting the detector Current = 1 nA (Check the baseline by changing the values if necessary.) Conditioning time Half a day (This time depends on the period during which the ECD has not been used.) ECD-2010 Exceed...

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