221-40463A

Electron Capture Detector

ECD-2010
USER’S MANUAL

READ AND UNDERSTAND THIS MANUAL

BEFORE OPERATION. SAVE THIS MANUAL.
Since a radioisotope is used as the raiation source, check the laws and regulations before installation.
Copyright © Shimadzu Corporation 2001. All rights are reserved, including those to reproduce
this publication or parts there of in any form without permission in writing from Shimadzu
Corporation.
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taken in its production will be corrected as soon as possible, but not necessarily immediately
upon detection.
Note that Shimadzu does not have any obligation concerning the effects resulting from the appli-
cation of the contents of this manual.
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 Precautions for Safe Operation

The ECD-2010 is a detector for Shimadzu gas chromatograph GC-2010.

For safe operation, observe the following precautions. If not observed, the safety may be compromised.

1. Use the unit only for the purpose for which it is intended.
2. Follow the procedures, warnings and precautions described in the mamual.
3. Do not disassemble or modify the unit.
4. For repairs, contact our sales office or service representative.

THREE CATEGORIES OF DANGER SYMBOLS ARE USED THROUGHOUT THE MANUAL.

WARNING Used for situations that may cause death or serious injury.

Used for situations that may cause slight injury or damage to the
CAUTION instrument.

NOTE Emphasizes additional information or provides tips for easier operation.

Read the safety information in the instruction manual of the gas chromatograph before using this unit.

I
1. Corrosive gas and dust
The vital section of the measuring circuit of this detector is shielded in a case.
In view of maintaining the service life and accuracy of the detector, avoid installing in a dusty or
corrosive environment.

2. Discharge of carrier gas

Connect a vinyl or teflon tube to the exhaust port (VENT) when using the detector, and set the other
end of the tube on the roof of the building or other place where no person is likely to come within 1 m
from the tube end.

3. Application name plates

Stick the name plates at the position shown below:

ECD VENT

ECD VENT
GC-2010

RADIOISOTOPE
NUCLIDE 63Ni

QUANTITY 370Mbq (10mCi)

RADIOISOTOPE
NUCLIDE 63Ni

QUANTITY 370MBq (10mCi)

II
 Contents
Precautions for Safe Operation

1 　Outline
1.1 Principle of the ECD (Electron capture Detector) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
1.2 Response Characteristics of the Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

2 　Parts List
2.1 Parts List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

3 　Basic Operation
3.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3.2 Gas used . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
3.3 Checking the glass insert and the injection inlet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3.4 Mounting the column . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
3.5 Setting the flow rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.6 Setting the flow rate of detector gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.7 Starting the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.8 Setting the detector temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.9 Setting the temperatures of the column oven and injection port . . . . . . . . . . . . . . . . . 15
3.10 Checking the baseline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.11 Setting the current value . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.12 Setting the range/attenuation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
3.13 Caution during analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
3.14 Stopping the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

4 　Key Operation
4.1 Setting the detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
4.2 Selecting the detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.3 Selecting the detector gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
4.4 Detector ON/OFF . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
4.5 Setting the range/attenuation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
4.6 Setting the current value . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
4.7 Zero adjustment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

5 　Service/Maintenance
5.1 Checking the ECD cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
5.2 How to Keep the ECD Cell Clean . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
5.3 Cleaning procedure for ECD Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
5.4 Actions to Be Taken in Case There Is the Doubt of Break . . . . . . . . . . . . . . . . . . . . . 44

ECD-2010 i
 Contents

6 　Troubleshooting
6.1 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
6.2 Error Message . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49

7 　Disuse
7.1 Cautions at Disuse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

8 　Maintenance Parts
8.1 Maintenance Parts List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53

9 　Specifications
9.1 Specifications of the ECD-2010 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

10 　Appendix
10.1 Structure of ECD Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
10.2 Calibration Curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
10.3 Conditioning of Equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

ii ECD-2010
 1 Outline

11.1
. 1.1 Principle of the ECD (Electron capture Detector)

Radiation (Beta-ray) from the radiation source (63Ni) sealed in the ECD cell ionizes an inert gas (N2). If a
pulse voltage is applied to the electrode in the cell, electrons are captured, allowing current to flow. If
electrophilic molecules enter the cell, the molecules absorb the electrons to be negatively ionized.
Negatively-charged molecules move more slowly than free electrons and take longer to reach the positive
electrode. Additionally, they are more likely to be bonded with positive ions again. Accordingly, the electrons
density in the detector drops so that a fewer number of electrons to be constant by increasing the pulse. The
total number of electrons to be captured in a unit time (and thus the current) can be maintained constant by
increasing the pulse frequency as the number of electrons decreases ; the variation in the number of pulses
is proportional to the density of the electrophilic molecules passing through the detector1).
1) R.J. Maggs et al., Anal. Chem. 43 (1971),1966
∆F = f - f 0 = Ka
f : Pulse frequency
f0 : Pulse frequency when carrier gas alone is allowed to flow (Basic frequency)
K : Constant determined by electron capture rate and other factors
a : Concentration of electron captivating substance

The construction of the system is schematically shown below.

Chromatopac

ECD cell

Pulse shaper
Carrier gas

System Block Diagram

Amplifier E compares the average pulse current from the ECD cell with reference current IR and outputs a
voltage to the voltage-frequency converter (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 1
 1 Outline

11.2
. 1.2 Response Characteristics of the Detector

The electron capture detector has an extremely peculiar response characteristic. The response varies largely
depending upon the kind of compound. Even with the same kind of compound, the response may change
largely with minor differences in the molecular structure, e.g., with racemates.
For reference, relative sensitivities for various compounds are listed below. For the same component,
response may vary depending upon the structure of the detector, temperature, applied voltage, etc.
Therefore, the figures below should be considered as just relative standards.

Relative sensitivity for various compounds (example 1)*

Compound Sensitivity (Unit is arbitrary)

1-chlorobutane 1.0
2-chlorobutane 2.0
1-chloro-2-methyl propane 1.7
2-chloro-2-methyl propane 12
1-chloropentane 1.0
1-chlorohexane 1.1
1-chloroheptane 1.5
1-chlorooctane 1.6
1, 2-dichloroethane 190
1, 4-dichlorobutane 15
1, 1-dichlorobutane 110
trans-1, 2-dichloroethylene 370
cis-1, 2-dichloroethylene 90
chloroform 6 × 104
carbon tetrachloride 4 × 105
1-bromopropane 255
1-bromobutane 280
bromocyclopentane 280
1-bromopropene-2 (allyl bromide) 4 × 103
1, 1-dibromoethane 1.1 × 105
1-iodobutane 9 × 104
benzene 0.06
toluene 0.2
2-fluorotoluene 0.55
4-fluorotoluene 0.55
chlorobenzene 75
bromobenzene 450
1-butanol 1.0
di-n-butyl ether 0.6
acetone 0.5
methyl butyrate 0.9
2, 3-butanedione 5 × 104
n-heptyl trifluoroacetate 4.5
n-propyl pentafluoropropionate 450

2 ECD-2010
 1 Outline
1.2 Response Characteristics of the Detector

Relative sensitivity for various compounds (example 2)**

Compound Sensitivity (Unit is arbitrary)

Hexane 0.9
Heptane 1.2
Octane 1.5
Decane 2.6
Chlorobenzene 5.5
Atrazine 3,000
Dichloroethane 20,000
Lead Tetraethyl 30,000
Benzophenone 100,000
2, 4D 125,000
Tedion 180,000
Malathion 250,000
Diethyl Maleate 550,000
Thioctane 600,000
2, 4, 5, T 800,000
Kelthane 1,600,000
DDD 2,000,000
D D T (para, para) 2,000,000
DDE 3,200,000
Heptachlor 4,800,000
Dieldrin 8,000,000
Aldrin 10,000,000
Lindane 11,000,000
Dibromoethane 11,000,000
Fluothane 16,000,000
Carbon Tetrachloride 400,000,000

* Phillippe Devaux, Georges Guiochon ; in “Advances in Gas Chromatography 1967”,A.Zlatikis,ed.

** K. P. Dimik, H.Hartmann ; presented at ACS Winter Meeting Cincinnati, Ohio January 13-18,1963

ECD-2010 3
 1 Outline
1.2 Response Characteristics of the Detector

4 ECD-2010
 2 Parts List

22.1
. 2.1 Parts List

This unit consists of the following contents. Confirm these contents.

List of parts for the ECD-2010

Control unit for the ECD-2010 (excluding the detector unit) :
part No. 221-47733-92

Part name Part No. Qty.

ECD control unit 221-48455-91 1
User’s manual (this document) 221-40463 1
APC flow controller 221-47743-91 1
Thermal insulation cup 221-44671 1
Label, RI 221-07755 2
Label, ECD vent 221-29747 1
Accessories and mounting parts for ECD-2010 221-48428-91 1
Consists of:
Screw (2-point Semus) M4 × 8 020-46147 2
Washer M4 023-66140-01 2
Column packing, aluminum 201-35183 1
Pipe insert, G6 201-36364-01 1
Pipe, MN2W-GN2W L350 201-48560-35 1
Molecular sieve filter 221-48602-91 1
MS-5A filter 201-36992-91 1
Signal cable 221-00816-03 1
Pipe MM-GF 300 mm 201-48561-30 1
Branch pipe MM-MF-MF 201-48386 1
Graphite ferrule adjuster for the ECD-2010 221-48610-03 1

ECD-2010 5
 2 Parts List
2.1 Parts List

6 ECD-2010
 3 Basic Operation

33.1
. 3.1 Introduction

Chapter 3 covers the basic operational procedure of the ECD.

The key sequence described in this chapter assumes that the parameters are set prior to the start of
the GC in accordance with “6. Analysis flow chart” in the instruction manual for the GC-2010 (CD-
ROM version). For the details of operations and key sequence for the gas chromatograph, refer to the
instruction manual for the GC-2010 (CD-ROM version).

■ Operation procedure for the ECD

<Key sequence>
Set the detector gas.
↓
Set the temperature of the injection port, column oven, and detector nearly at the room temperature.
↓
Press the [Start GC] key (PF menu) to start the control.
↓
Wait until the air in the ECD cell has been substituted by carrier gas and makeup gas.
↓
Set the detector temperature and current values.
↓
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 7
 3 Basic Operation

33.2
. 3.2 Gas used

Since the ECD is a detector with a high sensitivity, even slight impurities contained in the carrier gas may
affect the stability of the baseline.
A Gas Filter (option: 221-05619-01) and Oxygen trap (option: 221-46985-91) should be mounted along the
flow route to clear impurities from the carrier gas.
Both the carrier gas and make-up gas should meet the following purity standard:

■ Carrier gas (supply pressure : 300~980pa)

◎ Helium (most suitable) Purity 99.9999% or higher (applicable when purity is 99.999% or more)
○ Nitrogen (can be used) Purity 99.999% or higher (99.9999% or more is recommended)
○ Argon + Methane (5%) (can be used)

■ Make -up gas (supply pressure: 300~980kpa)

◎ Nitrogen (most suitable) Purity 99.9999% or higher (applicable when purity is 99.999% or more)
○ Argon + Methane (5%) (can be used)

8 ECD-2010
 3 Basic Operation

33.3
. 3.3 Checking the glass insert and the injection inlet

For the procedural details, refer to “12. Injection port” of the instruction manual for the GC-2010.

　WARNING
High temperature
You might suffer burns. Prior to start the work, check that the temperature at
each part is below 50°C.

　CAUTION
In order to prevent seizure or the like, do not turn the screw when the
temperature is high.

The glass insert for the injection port differs in shape depending on the injection port type and column used.
Check that the proper insert for the sample injection mode is selected, that the silica wool is positioned
properly, that there is no contamination, and that the O-ring for the glass insert has not yet deteriorated in
quality.

For split analysis For splitless/WBI

analysis

Fig. 3.3.1　Glass insert

Replace the injection inlet septum, in principle, when the number of injections reaches one hundred.

ECD-2010 9
 3 Basic Operation

33.4
. 3.4 Mounting the column

For the detailed procedure for mounting the column, refer to “4. Installing the column” in the instruction
manual for the GC-2010. The graphite ferrule shall be placed in the position (37 mm) indicated in the
following figure. This placement is possible using the supplied graphite ferrule adjuster (P/N. 221-48610-03)
for the ECD-2010.

Split/splitless ECD-2010
injection port

34mm 37mm

Graphite ferrule

Capillary column

Fig. 3.4.1　Position in which to retain the graphite ferrule

In order to prevent the ECD-2010 from being contaminated, connect the properly conditioned column.

■ Conditioning the column

Mount the column on the injection port only. Send the gas as in the analytical conditions. 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.

NOTE While the column is conditioned, the detector shall be sealed.

10 ECD-2010
 3 Basic Operation

33.5
. 3.5 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” of the instruction manual for the
GC-2010.

Fig. 3.5.1　

ECD-2010 11
 3 Basic Operation

33.6
. 3.6 Setting the flow rate of detector gas

Set the flow rate of the makeup gas in the following procedure:
Press the [DET] key to display the detector’s condition setting screen. If multiple detectors are mounted,
press the [Next Det] in the PF menu to go to the ECD screen.
Press the [Det Gas] key in the PF menu to go to the Makeup gas flow rate setting screen.
Enter the gas type and its flow rate.
Turn On the flow controller.
In case of the capillary column, set the flow rate of the makeup gas to 15~60 ml/min.

NOTE The detection sensitivity of the ECD-2010 depends upon the sample concentration in the carrier gas
containing the makeup gas. Unless the peak range expands, the sensitivity increases as the flow rate of the
makeup gas decreases. For the quantitative analysis, make sure to set the flow rate as that of the last analy-
sis.

Fig. 3.6.1　

12 ECD-2010
 3 Basic Operation

33.7
. 3.7 Starting the system

Press the [SYSTEM] key when the GC-2010 stops. The GC Start Sequence screen will appear.
Set the start time to 10 minutes or more.

　CAUTION
In order to avoid any damage to the ECD cell, set the start time so that the
detector temperature starts increasing after the air in the ECD cell has
entirely been substituted with the carrier gas and makeup gas. Before starting
the system, set the temperatures of the column oven and injection port to
nearly the room temperature (25°C).

After setting the parameters for starting the GC-2010, press the [Start GC] key in the PF menu. The GC will
start and the control will be performed for the temperatures at various parts and the flow rates of gases.
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.

Fig. 3.7.1　

ECD-2010 13
 3 Basic Operation

33.8
. 3.8 Setting the detector temperature

To set the temperature of the ECD detector, press the [DET] key to display the DET screen.

　CAUTION
In order to prevent the cell from being contaminated, set the detector
temperature to a value higher by at least 20°C than the maximum
temperature of the column oven during the analysis.

Using the cursor keys (UP and DOWN), move the cursor to the temperature row.
Enter a value with numeric keys and then press the [ENTER] key.
If the indicated detector is not the ECD-2010, press the [Next Det] key in the PF menu to change the
detector. (Pressing the toggle key allows you to change the PF menu.)

Fig. 3.8.1　

NOTE The detector temperature can be set via either the [SET] or [DET] screen. The value set on either screen will
be reflected on the other screen.

To check the baseline, set the range to ×10-1 (×2-3 for attenuation) and the current value to 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.
To change the range, move the cursor to the range on the [DET] screen. Using the LEFT or RIGHT cursor
keys, change the displayed range value and then press the [ENTER] key. (The attenuation can also be
changed in a similar procedure.)

14 ECD-2010
 3 Basic Operation

33.9
. Setting the temperatures of the column oven
3.9

and injection port

Press the [DET] key and check that the detector temperature has reached the set value.
After the detector temperature has reached the set value, it takes some time until the temperature in the ECD
cell is equilibrated. Wait for approximately 10~20 minutes and then set the temperatures of the column oven
and injection port.
For the detailed procedure, refer to “11. Column Oven” and “12. Injection Port” in the instruction manual for
the GC-2010.
For the injection port, press the [INJ] key to display the Injection Port screen and then set the temperature.
For the column oven, press the [COL] key to display the Column Oven screen and then set the temperature.
Pressing the [SET] key also allows you to set the temperatures. However, the temperature program cannot
be set.

　CAUTION
In order to prevent the ECD cell from being contaminated with matter eluting
from the column, maintain the detector at a temperature higher by at least
20°C than the column temperature.

Fig. 3.9.1　

ECD-2010 15
 3 Basic Operation

33.10
. 3.10 Checking the baseline

1. Set the attenuation of the Chromatopac (analog input) to 3 (2 ) and check that the baseline is
3

stabilized to the extent that becomes almost flat. For digital signals via the GCsolution or other, set the
full-scale value to 6.4×104 µV.

Fig. 3.10.1　Stabilized baseline

2. If the baseline is not stabilized as shown in Fig.3.10.2 or if it deflects from the range, see “6.1
Troubleshooting”.

Noise

Positive drift

Negative drift

Meander

Others

Fig. 3.10.2　Various abnormal baselines

Zero adjustment
Press the [MONIT] key and also press the [Zero Adj.] in the PF menu. The signal output will become 0 µV.
If the indication on the Chromatopac or other deviates from 0 µV after the zero adjustment has been
completed on the GC, additionally make the zero adjustment on the Chromatopac.
For further details, see “4.7 Zero adjustment”.

16 ECD-2010
 3 Basic Operation

33.11
. Setting the current value
3.11

The value for the current sent to the detector can be set in the range of 0.00 to 2.00 nA. As the current value
increases, the signal output becomes larger. Perform the analysis at a current value for which the zero
adjustment is possible.
For the high-sensitivity analysis, the current value may sometimes be set to 2 nA, but should normally be set
to 1 nA maximum. If the current value is too small, the output signal becomes so low that it cannot be
determined in some cases.
To change the current value, move the cursor to the current value on the [DET] screen using the UP or
DOWN cursor key. Enter a value and then press the [ENTER] key.

Fig. 3.11.1　

ECD-2010 17
 3 Basic Operation

33.12
. 3.12 Setting the range/attenuation

1. Analog output
If the analog output is connected to a data processing unit, two types of analog signal output, wide
range and linear range are available.
To connect the analog output to a data processing unit compatible with the wide range (the analog
input to the C-R7A, C-R7Aplus, or C-R8A), set the analog signal type to “Wide”. To connect it to any
other data processing unit, set the analog signal type to “Linear”.
If Wide is selected, no range selection is required. However, if the attenuation control on the data
processing unit does not work (e.g., an error peak occurs), the attenuation can be changed on the
[DET] screen. There are five attenuation levels from ×1 (2-0) to ×2-4. When the exponential value
increases by 1, the output becomes 1/2. Prior to using this function, calibrate the data processing unit.
(See “2.7 Connecting cables to the extended devices” of GC-2010 instruction manual.)
If Linear is selected, the range (amplification factor of the amplifier) can be set in five levels from ×1
(100) to x10-4. The range ×1 provides the largest amplification factor of the amplifier. The range ×10-1
provides 1/10 that amplification factor, the range ×10-2, 1/100, the range ×10-3, 1/1000, and the range
×10-4, 1/10000.
For the high-sensitivity analysis, therefore, use a small range (×1 or ×10-1). Otherwise, use a large
range (×10-2, ×10-3, or ×10-4).
Set the signal range of the detector and the analog signal type on the screen that is displayed by
pressing the [DET] key.

Fig. 3.12.1　

2. Digital output
If the digital output is connected a data processing unit compatible with digital signals (the digital input
to the GCsolution or the C-R8A), the digital signals are always output at ×1, which means that no
range selection is required.

18 ECD-2010
 3 Basic Operation

33.13
. 3.13 Caution during analysis

　CAUTION
Caution on sample
1. Clean up the sample as far as possible, if it is from a biological source,
and then inject it to the gas chromatograph.
2. Do not use a strong electrophilic compound, e.g., carbon tetrachloride or
chloroform as a solvent. This would cause the baseline to deflect from the
range, requiring longer time before the baseline becomes stable again.

NOTE 1. In general, the sensitivity becomes the highest when the column flow rate of the carrie gas plus the flow
rate of the makeup gas is 30~60 ml/min.
2. If helium is used as the carrier gas, the baseline level becomes too high when the wide-bore capillary
column or packed column in which the carrier gas flows at a high flow rate is used. 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 19
 3 Basic Operation

33.14
. 3.14 Stopping the system

1. For completely stopping the GC-2010

Select [Stop GC] from the PF menu on the screen that is displayed by pressing the [SYSTEM] screen.
The GC-2010 will enter into the stopping sequence in accordance with the set stop time and flow off
time. If the stop time is set, the temperature control, the background current control for the detector
will be stopped after the stop time has elapsed. If the program operation is used, they will be stopped
after the stop time has elapsed following the end of the program. The control of the carrier gas will
continue for the time period specified by the flow off time after the stop time has elapsed.
The flow off time means the time period from stopping the temperature control to stopping the carrier
gas. If this time period is short and if the supply of the carrier gas is stopped when the column oven
temperature remains high, the liquid phase in the column might be damaged. Set the flow off time
considering the time when the column temperature becomes low enough. The initial value is not set
for the flow off time, but set to “Cont.” Therefore, the carrier gas will continue to flow. When the
temperature at each part decreases sufficiently, stop the GC-2010 by turning OFF the power switch
located at the lower right part of the GC-2010.
For the details of stopping the GC-2010, refer to the instruction manual for the GC-2010.
To restart the GC-2010 that has been stopped by the above sequence, do as described in this
chapter. If the GC-2010 is stopped for a long period, close the main valves on the gas cylinders.

Fig. 3.14.1　

20 ECD-2010
 3 Basic Operation
3.14 Stopping the system

2. For continuous operation

For the continuous operation, the stopping operation is not required. In the split analysis, however, the
carrier gas can be saved if the split ratio is set to a smaller value.

NOTE The cell and flow path can be maintained to be clean by sending the makeup gas to the cell even if the ECD-
2010 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 21
 3 Basic Operation
3.14 Stopping the system

22 ECD-2010
 4 Key Operation

44.1
. 4.1 Setting the detector

4.1.1 Description on the screen

Press the [DET] key to display the main screen shown in Fig.14.1.1 and to set the detector
temperature, the detector gas flow rate, etc.
When the detector is configured in the line, the setting of the output signal appears in the lower
half portion of the screen.

For the detector signal output,

refer to “13.5 Setting the
Output Signals” of Instruc-
tion Manual for GC-2010.

Fig. 4.1.1　Main screen of [DET] key

4.1.2 Set item list

DETECTOR CONTROLLER
Selection: On/Off, Default: On
When a detector is set to “On”, its current and voltage are controlled.
When a detector is selected in a line and set to “On” here, the detector is used. However,
even if a detector is set to “Off” here, the gas flow and the temperature rises and reaches the
setup value if the detector is configured in a line.

TEMP
Range: 0.0 ～ 350.0°C, Default: 25.0°C
Set the detector temperature. Set usually the detector temperature to a value a little higher (by
approximately 30°C) than the column oven temperature (final temperature in temperature
program) so that adhesion of substances of high boiling point inside the detector can be
prevented. For setting of the maximum temperature, refer to “16.6.4 Setting of maximum
temperature” in “16.6 GC Configuration” of Instruction Manual for GC-2010.

ECD-2010 23
 4 Key Operation
4.1 Setting the detector

Current
Setting range: 0.00~2.00 nA, default value: 0.00 nA
Set the value for the current sent to the detector.

FILTER TIME CONSTANT

Selection: 4 ms/5 ms/10 ms/20 ms/50 ms/100 ms/200ms/500 ms/1 s/2 s, Default: 200 ms
This is the effect of the signal processing on the detector signal.
As the time constant is larger, noise is smaller and the peak height is lower.
Select the optimum value in accordance with the peak half width. (Refer to “13.4 Time
Constant of Filter Signal” of Instruction Manual for GC-2010.)

SIGNAL OUTPUT PORT

Selection: Off/Ch1/Ch2/Ch3/Ch4, Default: (Channel is automatically assigned.)
Set the channels for digital and analog signals output from the gas chromatograph. There are
four channels.
However, in the case of analog output, only Ch1 and Ch2 are offered as standard.

BACKGROUND SIG. SAVE

Selection: Off/Buff 1/Buff 2, Default: Off
You can store fluctuation of the base line as the background in the waveform memory of the
gas chromatograph.

BACKGROUND SIG COMP.

Selection: Off/Buff 1/Buff 2, Default: Off
You can subtract the base line stored as the background from the actual base line. By this
subtraction, stable base line can be output even if the base line considerably fluctuates.

DET SIG SUBTRACTION

Selection: Off/DET# 1/DET# 2/DET# 3/DET# 4, Default: Off
You can subtract the signal output from another detector from the signal output from the
detector. This function is mainly used in a dual column flow line to subtract the data acquired
by analysis without sample injection from the data acquired by analysis with sample injection
so that the background is eliminated.
For the details of “SIGNAL OUTPUT PORT”, “BACKGROUND SIG. SAVE”, “BACKGROUND
SIG COMP.” and “DET SIG SUBTRACTION”, refer to “13.5 Setting the Output Signals” of
Instruction Manual for GC-2010.

SIGNAL RANGE
Selection: ×1/×10-1/×10-2/×10-3/×10-4, Default: /×10-1
You can multiply the analog signal by the coefficient “10-x” when the analog signal type is
linear. If the peak is saturated in the data processing unit, change the setting from “×1” to “×10-
1”, from “×10-2” to “×10-3”, for example. In case of the digital signal, the signal is always output

with “×1”.

SIGNAL ATTENUATION
Selection: ×1/×2-1/×2-2/×2-3/×2-4, Default: /×2-1
You can multiply the analog signal by the coefficient “2-x” when the analog signal type is wide.
If the peak is saturated in the data processing unit, change the setting from “×1” to “×2-1”, from
“×2-2” to “×2-3”, for example. In case of the digital signal, the signal is always output with “×1”.

24 ECD-2010
 4 Key Operation
4.1 Setting the detector

ANALOG SIGNAL TYPE

Selection: Linear/Wide, Default: Linear
Set this item when the GC is connected to the chromatopac in the analog format.
When the GC is connected to the C-R8A, the value set here does not effect the signal
because they are connected in the digital format via an RS-232C cable.
Wide ... Select it when connecting the GC to the C-R7A/C-R7A plus.
The signal raised to the “1/2” power is output from the GC, then the signal
received by the chromatopac is squared.
When connecting the GC to the C-R7A/CR-7A plus for the firs time or replacing
the chromatopac, set the detector signal output to “Off” and perform calibration.
For the calibration procedure, refer to “2.6 Connection of External Unit” of
Instruction Manual for GC-2010.
Linear ... Select it when connecting the GC to any chromatopac other than the C-R8A/C-
R7A/C-R7A plus.
When connecting the GC to the C-R7A/C-R7A plus and setting “ANALOG
SIGNAL TYPE” to “Linear”, the optional signal cable (linear, P/N 221-47251-92) is
required.

4.1.3 PF menu list

PF menu Description
Det Gas Sets the flow rate of makeup gas, if the advanced Pressure Control (APC) is installed.
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 25
 4 Key Operation
4.1 Setting the detector

4.1.4 Checking the installation state setting

Pressing the [FUNC] key and selecting “7. Service/Maintenance” in the screen that appears
displays the sub-screen shown in the figures.

1. Installation state setting (position)

Pressing the numerical key [1] or using the cursor key (up/down), place the cursor on “1.
Installation (Position)” and press the [ENTER] key.

Fig. 4.1.2　

1) Check that the ECD-2010 has been recognized.

When ECD is not displayed, control unit may not be installed correctly or a failure may
have occurred.
2) Confirm that the installation position of the unit is set correctly.
When changing, move the cursor to the applicable column using the cursor keys (up/
down), input numerical values, and press the [ENTER] key.
The relation between the installation position and the number is as follows:

26 ECD-2010
 4 Key Operation
4.1 Setting the detector

(0 = Not installed, 9 = Installed at the position other than those in the figure.)

8 4

7 3
6 2
1

Top view

Fig. 4.1.3　

2. Setting the installation state (piping)

If “7. Service/Maintenance” is selected on the screen that is displayed by pressing the [FUNC]
key, the subscreens shown below will appear. Press the numeric key [2], or position the cursor
on “2. Installation (Piping)” using the cursor keys (UP and DOWN) and then press the
[ENTER] key. Check that the flow controller for the detector gas (makeup gas) is set properly.

Fig. 4.1.4　

Cont. Type
The control unit type is automatically recognized and displayed. When this is not displayed,
the control unit may not be mounted correctly or a failure may have occurred.

ECD-2010 27
 4 Key Operation
4.1 Setting the detector

Slot No.
Select the APC slot number connected to the detector.
The DET APC No. and Unit type are automatically displayed when SLOT is set.
Also, “APC (1ch)” is used for ECD.

Heater port
This is the temperature control port of the detector to which flow controller set in the slot is
connected.
Set DET 1 when the DET1 is connected to the ECD detector and DET2 when connected to
DET2.
For the details, refer to “16.7 Service and maintenance” in GC-2010 Instruction Manual (CD-
ROM version).

4.1.5 Checking the detector setting of line configuration

Press the [SET] key and display the SET key screen.
Press [Line Confg] of the PF menu and display the sub-screen of the line configuration.

Fig. 4.1.5　

Confirm that ECD in the detector column is set to an appropriate line.

When changing the line configuration, move the cursor to the ECD line using the cursor keys (up/
down), select the line, and determine the selection by pressing the [ENTER] key.
For the details, refer to “8. Setting the Analytical Parameters and File Management” in the GC-
2010 Instruction Manual (CD-ROM version).

28 ECD-2010
 4 Key Operation

44.2
. 4.2 Selecting the detector

The key operation and the screen display when selecting the detector are as follows:
Pressing the [DET] key displays the setting screen of the detector. When more than one detector is loaded,
the setting screen of the currently selected detector will be displayed.
Press the toggle key to select the PF menu. Pressing the [Next Det] can select the other detectors.
When no detector is connected, pressing the [DET] displays “Detector is not installed”.
When changing from FID of DET#1 to ECD of DET#2, the screen is changed as follows:

Fig. 4.2.1　

ECD-2010 29
 4 Key Operation

44.3
. 4.3 Selecting the detector gases

Press the [DET] key to display the [DET] screen. Select Detector Gas from the PF menu. The [DET Gas]
screen will appear.
Set the type of gas to “N2”.
Set the flow rate of the makeup gas using the following values as guidelines:

■ For the capillary column:

makeup gas (N2) -- 15 to 40 ml/min (50 to 100 kPa)

■ For the packed column:

makeup gas (N2) -- 5 to 10 ml/min (20 to 40 kPa)

Fig. 4.3.1　

PF key
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

NOTE 1. The detection sensitivity of the ECD-2010 depends upon the concentration of the sample in the carrier
gas (including the makeup gas). Therefore, the sensitivity increases, as the flow rate of the makeup gas
becomes lower, unless the peak range expands.
2. To purge the detector connecting part of the column, send the makeup gas to even the packed column.
3. If the detector gas is stopped, it will take longer time before the baseline becomes stable when the
system is restarted. It is recommended that the makeup gas be continuously sent even if the GC stops.

30 ECD-2010
 4 Key Operation
4.3 Selecting the detector gases

Flow rate program for detector gases

The flow rate program may be set for a maximum of seven stages.
To set the program, do as in the case with the carrier gas program.
For further information, refer to “13.2.3.4 Flow rate program for detector gas” of the instruction manual
(CD-ROM version) for the GC-2010.

Fig. 4.3.2　

Under the general analytical conditions, the flow rate program for the detector gases is not necessary to use.

ECD-2010 31
 4 Key Operation

44.4
. 4.4 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. 4.4.1　

32 ECD-2010
 4 Key Operation

44.5
. 4.5 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 ×10-1. For the high-sensitivity analysis, use
×1. If the analog signal type is Wide, use ×2-1.
Digital signals are output as ×1 regardless of the above setting.

Fig. 4.5.1　

ECD-2010 33
 4 Key Operation

44.6
. 4.6 Setting the current value

The value for the current sent to the detector can be set in units of 0.01 nA in the range of 0.00 to 2.00 nA.
The default value is 0.00 nA. The output signal increases as the current value becomes larger. However, the
sensitivity remains almost unchanged because 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. 4.6.1　

34 ECD-2010
 4 Key Operation

44.7
. 4.7 Zero adjustment

Zero adjustment procedure

1. Select the detector to perform zero adjustment.

2. Perform key operation.
3. Make zero adjustment of the data processing unit. (For the operation method, refer to the instruction
manual of the data processing unit such as Chromatopac.)

Selecting the detector to perform zero point adjustment.

Zero adjustment is performed on the Monitor screen.
This section describes zero adjustment only. For the details of the monitor screen, refer to “9. Monitor” in
the GC-2010 Instruction Manual.
Pressing the [MONIT] key displays the main screen. When the displayed line configuration does not
include the ECD, press [Chng Line] of the PF menu and change the line.

Fig. 4.7.1　

ECD-2010 35
 4 Key Operation
4.7 Zero adjustment

Key operation No. 1: Automatic zero adjustment

Pressing the [Zero Adj] in the PF menu changes the display on the screen to 0 µV and the baseline moves
to the zero point of the GC. However, depending on the range of the detector and the attenuation of the
Chromatopac, baseline cannot be accommodated within the screen of Chromatopac.

Fig. 4.7.2　

[Zero adj.]

Z key on the
Chromatopac

Zero point on
the Chromatopac

If the baseline is stable,

the analysis possible.

36 ECD-2010
 4 Key Operation
4.7 Zero adjustment

Key operation No. 2: Zero point adjustment

Pressing [Up][Down] of the PF menu changes the baseline level upward/downward.

Fig. 4.7.3　

Example: Chromatopac screen

[Down]

Z key on the
[Up] Chromatopac

Zero point on
the Chromatopac

The baseline has decreased to the The zero point is If the baseline is stable,
negative side since the [Down] key adjusted for the the analysis is possible.
has been held down too long. Chromatopac.

ECD-2010 37
 4 Key Operation
4.7 Zero adjustment

Key operation No. 3: Releasing zero adjustment

Pressing the [Zero Free] of the PF menu returns the baseline to the level before zero adjustment is
performed.

Fig. 4.7.4　

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”.

38 ECD-2010
 5 Service/Maintenance

55.1
. 5.1 Checking the ECD cell

If the sample or other accumulates on the inside of the ECD cell, the baseline level becomes higher. Even in
this case, the analysis can be performed so far as the baseline does not deflect from the range when the
[Zero Adj] key is pressed. If the current value is decreased, the baseline can be lowered. In this case,
however, the output signal (peak) becomes smaller.

For the daily service, check the ECD cell for contamination in the following steps:

1. Set the temperatures of the column mounted and other parts, the flow rate, and the current value as
during the analysis.

2. Wait until the baseline has become stable enough.

3. Press the [MONIT] key to display the MONIT screen (if the ECD-2010 is not included in the displayed
line, press the Chng Line key in the PF menu to change the displayed line).

4. Press the [Zero Free] key in the PF menu and then read the detector signal level indicated.
5. In principle, the signal level (µV) in the above step 4. falls below the following value against the set
current value, the cell contamination is regarded as within the acceptable level:

Set current value (nA) × 90000 (e.g., the set current value is 1 nA, the limit is 90000 µA).

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.

When the standard diagnostic function is used:

1. Press the [DIAG] key to display the Diagnosis menu.

2. Select “1.Standard Diagnosis”
3. Press the [DiagParam] in the PF menu to display the “Diagnosis Parameters” screen.
4. Move the cursor to the ECD Frequency item and then set it to “Yes.”
All the items that are set to “Yes” will be diagnosed. To check the ECD-2010 only, set all the other
items to “No.”

5. Press the [Return] key in the PF menu. You will return to the Main screen for the standard self-
diagnosis. Press the [StartDiag] key in the PF menu to start the diagnosis.

6. When the diagnosis is completed, the comprehensive diagnostic result and the number of anomalies
will be displayed.

7. If the diagnostic result for the ECD frequency is Not Good, it is recommended that the cell be cleaned
(the radiation source be replaced).
(see “5.3 Cleaning Procedure for ECD Cell.”)
For the details of the self-diagnosis, refer to Chapter “14. Diagnosis” in the instruction manual for the
GC-2010 (CD-ROM version).

NOTE In the standard self-diagnosis, the default value for the threshold of the ECD frequency is 40 kHz at 2 nA.
This value can be changed if the standard value for the system check is selected in the system configuration
of the GCsolution for the ECD-2010. However, it cannot be changed on the GC-2010 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 39
 5 Service/Maintenance

55.2
. 5.2 How to Keep the ECD Cell Clean

The following cautions should be exercised in order to keep the ECD cell clean:

1. Use a column with excellent heat resistance

A major factor causing contamination of the ECD cell is the accumulation of the liquid phase of the
column. Use of a column with excellent heat resistance is recommended. Also, the life of the ECD cell
can be lengthened when it is used at a temperature 20~30°C lower than its max. temperature.

2. Use a column with less quantity liquid phase

Use of a column with less quantity liquid phase is also recommended to prevent accumulation of the
liquid phase on the ECD cell. Although capillary columns are hardly affected, care should be
exercised when using a packed column.

3. Use a column which has been sufficiently conditioned

The column to be used should be sufficiently conditioned in order to prevent impurities from
accumulating on the ECD cell. It is recommended that the column be conditioned without connecting it
to the ECD cell in order to prevent deterioration of the operational life of the ECD cell.

4. Condition the injection port sufficiently

The injection port should also be sufficiently conditioned, in the same way as the column in step (3)
above. Check the injection port (glass insert) for contamination and carry out sufficient conditioning.
(Refer to “10.3 Conditioning of Equipment”.)

5. Reduse impurities in the carrier gas and make-up gas

The carrier gas and make-up gas containers of the ECD should be of high purity. Flow route parts
(pipes, flow controller, etc.) should also be clean. A gas filter and oxygen trap are effective for
removing impurities.

6. Condition the ECD cell periodically

Condition the ECD cell periodically. When conditioning, the temperature of the ECD cell should be set
as close to the max. operation temperature, 350°C, as possible (for instance 340°C). (Refer to “10.3
Conditioning of Equipment”)
When conditioning the ECD cell with the column connected, the temperature of the column oven
shoud be one given below:

Capillary column : Max. temperature

Packed column : (Max. temperature) -30°C

When a packed column with a low boiling point of the liquid phase is used at a high temperature,
conditioning the ECD cell immediately after use is an effective method for extending the operational
life of the ECD cell.

7. Set the detector temperature to a value higher than that of the column oven.
The liquid phase of the column does not accumulate on the ECD cell if the detector temperature is
higher than the column oven temperature. Set the detector tremperature to a value 20~50°C higher
than that of the column oven. However, beware that the max. operation temperature of the ECD is
350°C. (Refer to “3.8 Setting the detector temperature”.)

40 ECD-2010
 5 Service/Maintenance
5.2 How to Keep the ECD Cell Clean

8. In case of contimuous operation, lower the temperature.

Many analyses carried out using the ECD cell are contimuous. In such cases, if the analysis is carried
out with the column oven heated to a high temperature, the liquid phase, in particular of the packed
temperartures of the column oven and the injection port be lowered if possible.
However, neither the carrier gas nor the make-up gas shoud be stopped. (Refer to “3.14 Stopping the
system”.)

9. When ECD is not used

When the ECD is not used, close the column connection of the ECD cell and supply the make-up gas.
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 41
 5 Service/Maintenance

55.3
. 5.3 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 our company for cleaning (repair) of the ECD cell in the following procedure:

　CAUTION
For the mounting and removing the ECD unit, contact our service engineer.

1. Ask our Sales office for a “Request for a Cleaning ( Repairing ) ECD Cell” slip.
2. Write the necessary information including your special request on the slip and send it to us (Sales
office).

3. Remove the ECD unit from the gas chromatograph main body.
4. The ECD unit must be sent by the user himself directly to our office by mail according to the law.
(For the mailing method and the address, please contact our Sales office.)

5. The ECD unit sent from you will be cleaned (or repaired)
by us according to the information on the slip.

6. After having been cleaned or repaired, the ECD unit will be sent back to you by mail.
7. Mount the ECD unit on the main body.
NOTE In cleaning the ECD cell, it is unavoidable to handle the nonsealed source. Therefore, if the user wants to
clean the cell on his side, it is essential that he observe the applicable national, state and/or local laws and
regulations regarding the handling of radioactive materials.

42 ECD-2010
 5 Service/Maintenance
5.3 Cleaning procedure for ECD Cell

User Shimadzu corporation

Request for cleaning.

Call us.
Branch office or agent

Request for cleaning

(Repairing) ECD cell

Mail the request slip

Fill out the slip

We will explain how to pack

and mail the ECD unit.

Request
GC-2010 slip

Remove the ECD unit. Use the box the ECD unit originally
came in for mailling.

Pack

Mail Shimadzu corporation

RI acceptance card is sent.

RI
acceptance
card
Cleaning

Repair

Mail

GC-2010

Remount the ECD unit.

Completed.

Fig. 5.3.1　Cleaning the ECD cell (replacing the radiation source)

ECD-2010 43
 5 Service/Maintenance

55.4
. Actions to Be Taken in Case There Is the
5.4

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.

NOTE Refer to “7 Disuse”.

44 ECD-2010
 6 Troubleshooting

66.1
. 6.1 Troubleshooting

This chapter covers causes of and countermeasures against troubles encountered when using the ECD.
Troubles which are attributable to the gas chromatograph main unit are covered in “Troubleshooting” in the
instruction manual of the gas chromatograph.
If a trouble cannot be cleared by the countermeasure given hereafter, or if a troubles other than outlined in
this chapter occurs, contact Shimadzu office or agent which is nearest to you.

1. Abnormal baseline
■ Significant noise occurs in the baseline.

Noise

Cause Countermeasures
The electrical connector is not securely connected. Check the connector and connect securely.
There is a large quantity of impurities in the carrier • Purge the air inside the flow line completely. (Refer
gas or make-up gas. to “10.3 Conditioning of Equipment”)
• Replace the filter (molecular sieve filter, gas filter
or oxygen trap).
• Replace the plumbing parts.
• Replace the gas container, changing to a gas of
higher purity.
Gas leakage Check for gas leakage and correct any joints from
which gas is leaking.
The cell is contaminated. Check the cell for contamination. If necessary, send
the ECD unit to our Company for cleaning. (Refer to
“5. Service/Maintenance”.)

ECD-2010 45
 6 Troubleshooting
6.1 Troubleshooting

■ Baseline drift, meander, etc.

(Positive) drift (Negative) drift Meander Others

Cause Countermeasures
Air is trapped in the flow line. Purge the air completely. (Refer to “10.3 Conditioning
of Equipment”.)
The carrier gas or make-up gas is not flowing and air Correct the flow conditions of the carrier gas or make-
is mixed in. up gas.
Injection port (glass insert) or column is contaminated. • Clean the glass insert or replace it. (Refer to “3.3
Checking the glass insert and the injection inlet”.)
• Condition the column. (Refer to the instruction
manual of the gas chromatograph.)
Temperature of each section is unstable. Monitor the temperature of each section on the
monitor screen ([MONIT] key).
Contact our branch office or agent if the temperature
will not stabilize.
The flow rate is unstable. Monitor the pressure and flow rate on the monitor
screen ([MONIT] key).
Contact our branch office or agent if the temperature
will not stabilize.
The cell is contaminated. Check the cell for contamination. If necessary, send
the ECD unit to our company for cleaning. (Refer to
“5. Service/Maintenance”.)

2. Zero adjustment does not work.

Exceeding the limit.

Cause Countermeasure
Air is trapped in the flow route. Purge the air completely. (Refer to “10.3 Conditioning
of Equipment”.)
The carrier gas or make-up gas is not flowing and air Correct the flow conditions of the carrier gas or make-
is mixed in. up gas.
The cell is contaminated. Check the cell for contamination. If necessary, send
the EDC unit to our company for cleaning. (Refer to
“5. Service/Maintenance”.)

46 ECD-2010
 6 Troubleshooting
6.1 Troubleshooting

3. Peak is too small (or the sensitivity is too low.)

Cause Countermeasures
The carrier gas is leaking. Check for gas leakage and correct any piping joints
from which gas is leaking.
The split ratio is too large. (in case of split analysis) Reduce the split ratio.
The quantity of the sample injected is too small, or the Increase quantity or concentration of injected sample.
sample concentration is too low.
The value of current, range or attenuation is inappro- Set the range or attenuation to ×1 or current.
priate.
The capillary column has been connected in the Mount the column in the correct way.
wrong way. (Refer to “3.4 Mounting the column”.)
An incorrect column is used. Replace the column in the correct one, taking the
polarity into consideration.
There is a large quantity of impurities in the carrier • Purge the air inside the flow route completely.
gas or make-up gas. (Refer to “10.3 Conditioning of Equipment”.)
• Replace the filter (molecular sieve filter, gas filter
or oxygen trap).
• Replace the plumbing parts.
• Replace the gas container, changing to a gas of
higher purity.
The cell is contaminated. Check the cell for contamination. If necessary, send
the ECD unit to our company for cleaning. (Refer to
“5. Service/Maintenance”.)

ECD-2010 47
 6 Troubleshooting
6.1 Troubleshooting

4. The linearity of the calibration curve has become significantly poor. (Refer to “10.2 Calibration
Curve”.)

Calibration curve

Cause Countermeasures
There is a large quantity of impurities in the carrier • Purge the air inside the flow route completely.
gas or make-up gas . (Refer to “10.3 Conditioning of Equipment”.)
• Replace the filter (molecular sieve filter, gas filter
or oxygen trap).
• Replace the plumbing parts.
• Replace the gas container. (changing to a gas of
higher purity.)
The column is contaminated . • Condition the column. (Refer to the instruction
manual of the gas chromatograph.)
The cell is contaminated. Check the cell for contamination. If necessary, send
the ECD unit to our company for cleaning. (Refer to
“5. Service/Maintenance”.)

5. Other abnormal phenomena

As for the phenomena shown below , refer to “Troubleshooting” in the instruction manual of the gas
chromatograph.

○ The pressure meter does not indicate the set value.

○ Gas leakage does not stop.
○ 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.

48 ECD-2010
 6 Troubleshooting

66.2
. 6.2 Error Message

Error messages specific to the ECD are explained in this section. As for the error messages relating to the
gas chromatograph main unit , refer to “19.2 Error Messages” in the instruction manual of the gas
chromatograph.

■ OVER TEMP error

The DET temperature has exceeded the upper limit.

If the unit for which the temperature is controlled exceeds the upper limit for its operating temperature, the
confirmation screen appears prompting you to reset the error with the above message displayed.

When the ECD is used, the max. temperature of the detector is set to 350°C or less. For the ECD, if the
detector temperature exceeds 350°C, the safety function operates automatically and it becomes OVER
TEMP. error.
Therefore, if an attempt to set the detector temperature to over 350°C, this OVER TEMP error returns.
Beware that, even when the detector temperature has been set to less than 350°C, the temperature may
exceed 350°C momentary on the way to the set value.

If this error occurs, move the cursor to “Ignore Error” and then press the [ENTER] key. Eliminate the cause
of the error by changing the settings or taking any other action. Several 10 seconds after the [ENTER] key
has been pressed, the confirmation screen appears. Position the cursor on “Reset Error” and then press
the [ENTER] key.
If you return to the confirmation screen when you are changing the settings, select “Ignore Error” again.

ECD-2010 49
 6 Troubleshooting
6.2 Error Message

50 ECD-2010
 7 Disuse

77.1
. 7.1 Cautions at Disuse

When disusing the used ECD etc., you must take legal administrative procedures at the same time. 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.

NOTE When removing the ECD from the gas chromatograph, contact our service engineer.

* When removing the ECD unit, plug the hole with the heat insulating material which was cut off at
installation.

ECD-2010 51
 7 Disuse
7.1 Cautions at Disuse

52 ECD-2010
 8 Maintenance Parts

88.1
. 8.1 Maintenance Parts List

Part name Part No. Remarks

Silicon rubber septum (20 pcs.) 201-35584 Injection port septum
Glass insert (for split injection) 221-41444-01 For split injection method
Glass insert (for splitless injection) 221-48335-01 For splitless injection method
Inert silica wool (2 grams) 221-48600 Stuffing for glass insert
Fluoride rubber O-ring (5 pcs.) 036-11203-84 For fitting the glass insert
Graphite ferrule 0.5 mm (10 pcs.) 221-32126-05 For mounting the capillary column
Graphite ferrule 0.8 mm (10 pcs.) 221-32126-08 For mounting the wide-bore column
Aluminum packing (500 pcs.) 201-35183-84 Packing for the piping joint

ECD-2010 53
 8 Maintenance Parts
8.1 Maintenance Parts List

54 ECD-2010
 9 Specifications

99.1
. 9.1 Specifications of the ECD-2010

Type : Frequency-controlling , constant current type

Radiation source : 63Ni 370MBq

Cell : Coaxial type electrode with purging line

Cell current : 0.00 - 2.00 nA
Linearity : 104 (with γ - BHC)
Detection limit : 8 fg / s
Max. temperature : 350°C
Range : 5 steps of ×1, ×10-1, ×10-2, ×10-3, and ×10-4 (at analog and linear output)
Attenuation : 5 steps of ×1, ×2-1, ×2-2, ×2-3, and ×2-4 (at analog and wide output)

ECD-2010 55
 9 Specifications
9.1 Specifications of the ECD-2010

56 ECD-2010
 10 Appendix

1010.1
. Structure of ECD Cell
10.1

Electrode

Radioactivity mark
mechanism confirmation mark

To VENT

Radiation source

Input of make-up gas

Heating block
ECD cell body

Capillary adaptor

Fig. 10.1.1　Structure of the ECD unit

ECD-2010 57
 10 Appendix

1010.2
. 10.2 Calibration Curve

This chapter covers the explanation of linearity of calibration curve which has been described in 6.1
“Troubleshooting”.

Calibration curve
The “Calibration curve” refers to the graph shown in Fig.10.2.1. this graph shows the relationship between
the sample quantity and the height of the peak.

Dynamic range
The “linearity of calibration curve” refers to in what range the graph can be regarded as the straight line.
This range is called as the dynamic range. For instance in Fig.10.2.1, the graph between the sample
quantity of 10-1 pg to the sample quantity 103 can be regarded as the straight line. Therefore, the dynamic
range in this case is 103 / 10-1 = 104.

Quantativity
In the range in which the calibration curve appears as straight line, the peak height is proportional to the
sample quantity. It means that the quantitative analysis cad be performed within this range. Note that the
quantitative analysis cannot be performed out of this range.

Characteristics of the ECD

Fig. 10.2.1 is an example of the calibration curve. This calibration curve is one when the ECD cell is in the
best condition .

Dynamic range
6
10

5
10
Peak height

4
10

3
10

2
10
-1 0 1 2 3 4
10 10 10 10 10 10 (Pg)

Sample quantity
Detection limit

58 ECD-2010
 10 Appendix

1010.3
. Conditioning of Equipment
10.3

After the installation of equipment or after the replacement of pipings, air is trapped inside the flow line. If air
is mixed in the gas inside the flow line, the base line, the base line connot be stabilized and analysis cannot
be performed correctly. Equipment must be conditioned prior to starting analysis. Given in this section is an
example of settings of equipment conditioning . As for the details of the operational procedure, refer to “3.
Basic Operation”.
It is recommended to condition the equipment in the following settings :

1. Glass insert in the injection port

Same glass insert as that used for analysis
(Confirm the kind glass inserts. Check the glass insert for contamination and for damage.)
(Refer to “3.3 Checking the glass insert and the injection inlet”.)

2. Column
Use of an empty column (column without liquid phase) is recommended.
(to prevent the liquid phase of the column from being accumulated on the ECD cell)
When a normal column is connected, use a column with an excellent heat resistance Also, a packed
column should not be used for the conditioning of equipment since its liquid phase quantity is large.

■ In case of a capillary column :

A fused silica tube (option : for instance FQ tube 0.2 mmID×2 m, P/N 221-25964-02) is conveniently
used.

■ In case of a packed column :

Pipe MF-MF (option:P/N 201-48555-**, -** is the length. For instance if the pipe is 30 cm, it is
expressed as -30 cm, If it is 1m. It is expressed as-00.) It can be used as a empty column.

3. Temperature setting
Column over temperature : 340°C (empty column)
Injection port temperature : 340°C
Detector temperature : 340°C

NOTE When a normal column is connected, the column oven temperature should be set lower than max.
temperature of the column by 30°C and more.

4. Flow rate setting

The flow rate of both carrier gas and make-up gas should be set to the same rates as those for
analysis .

NOTE When the FQ tube (0.2 mmID×2 m) mentioned above is connected, conditioning can be performed if the flow
rate is within the control range of the flow controller and if the carrier gas is flowing to the column.

5. Detector settings
Range=1 , Current=1 nA
(Check the baseline by changing the values if necessary.)

6. Conditioning time
~half a day
(This time depends on the period during which the ECD has not been used.)

ECD-2010 59
 10 Appendix
10.3 Conditioning of Equipment

60 ECD-2010