DETECTORS

Electron Capture Detector - ECD

OVERVIEW
The Electron Capture Detector (ECD) is selective to electronegative compounds, especially chlorinated,
fluorinated, or brominated molecules. It is sensitive to some of these compounds in the parts per trillion (ppt)
range. The ECD detector requires nitrogen or argon / 5% methane (P5) to operate. The ECD detector is
mounted immediately adjacent to the right rear column oven wall on your SRI GC chassis. Two BNC cables
connect the anode and cathode, respectively, to the ECD amplifier. The ECD detector consists of a stainless
steel cylinder containing 5 millicuries of radioactive Nickel 63 in an oven enclosure that is thermostatically
controllable from ambient temperature to 375oC. Since the detector contains only 5 millicuries of Nickel-63,
the ECD is covered by a “General License” requiring a periodic wipe test and the filing of a form with your
state’s Department of Health. The documentation necessary to authorize your possession of a radioactvie
source is included in the ECD manual from Valco, the manufacturers. This documentation transfers possession
of the ECD directly to you from Valco; SRI provides the ECD installation service and the GC. There are four
important documents to look for: 1) Certification of Sealed Source, 2) Conditions for Acceptance of a Generally
Licensed Device, 3) Test Specifications, and 4) Record of Source
Transfer. Valco may print your address on the multiple copies of
the Record of Source Transfer, which are to be completed by
you and filed with the appropriate state and local authorities.
The other documents remain with the ECD detector, and
Parts kit
containing
are necessary to prove authorized possession of the ECD.
test resistor
ECD 1
Detector

ECD-equipped SRI GC Trimpot setpoints

2

It is imperative to 4
complete the Record of
Source Transfer and forward it to
proper authorities, and to familiarize
yourself with the requirements of your
Your name &
General License. You must also keep
address here
on file the Cerification of Sealed
Source and Test Specifications,
which are proof that your
ECD detector meets
regulations.
Close-up view of the ECD detector
on an SRI GC
 DETECTORS
Electron Capture Detector - ECD

Theory of Operation

The radioactive Nickel 63 sealed inside the ECD detector emits electrons (beta particles) which collide
with and ionize the make-up gas molecules (either nitrogen or P5). This reaction forms a stable cloud of free
electrons in the ECD detector cell. The ECD electronics work to maintain a constant current equal to the
standing current through the electron cloud by applying a periodic pulse to the anode and cathode. The
standing current value is selected by the operator; the standing current value sets the pulse rate through the
ECD cell. A standing current value of 300 means that the detector electronics will maintain a constant current
of 0.3 nanoamperes through the ECD cell by periodically pulsing. If the current drops below the set standing
current value, the number of pulses per second increases to maintain the standing current.

ECD Detector Operational Diagram

Sample-laden
carrier gas Makeup gas Standing
inlet inlet current (equal
and opposite to
the cell current)
ECD cell
Electron cloud
ANODE

Nickel 63 foil
Integrating amplifier
CATHODE
Gas outlet

Voltage-controlled
variable frequency
Frequency / voltage Analog voltage output pulser
Offset control converter to PeakSimple data
system

When electronegative compounds enter the ECD

cell from the column, they immediately combine with Example Pulse Trains
some of the free electrons, temporarily reducing the
number remaining in the electron cloud. When the
electron population is decreased, the pulse rate is
increased to maintain a constant current equal to the Detector electronics pulse to maintain the
standing current. The pulse rate is converted to an standing current
analog output, which is acquired by the PeakSimple
data system. Unlike other detectors which measure an
increase in signal response, the ECD detector electronics The pulse rate is increased in the presence of
measure the pulse rate needed to maintain the standing electronegative compounds
current.
 DETECTORS
Electron Capture Detector - ECD

Expected Performance

ECD Noise Run

Column: 15m MXT-5 capillary

Carrier: Helium @ 10mL/min
Makeup: Nitrogen @ 60mL/min
ECD Temp: 250oC
ECD standing current: 300
Offset before zeroing the data
system signal: 280mV

ECD noise averages less than 1mV from peak to peak

ECD Pesticide Analysis

Sample: 1µL 200ppb chlorinated

pesticides
Column: 15m MXT-5 capillary
Carrier: Helium @ 10mL/min
Makeup: Nitrogen @ 60mL/min
ECD temp: 250oC
ECD standing current: 300

Results:
Component Retention Area
Pesticides 2.850 45792.4350
DETECTORS
Electron Capture Detector - ECD

General Operating Procedure

The following suggestions are specific to your SRI ECD-equipped GC. Consult the Valco ECD detector
manual for carrier gas purity requirements, carrier gas system configuration, and other general ECD detector
information. Keep in mind that the electronics shematics in the Valco manual do not apply to your ECD-
equipped SRI GC.

1. Cap off the carrier inlet to the ECD cell (in the column oven).
2. Connect the makeup gas and let it flow through and purge the ECD cell.
Makeup flow is 40-100mL; typically 60mL.
3. Heat the ECD detector to 150oC to verify that the baseline noise and offset
are normal. 150oC is hot enough to evaporate off water but low enough to avoid
oxidation of the nickel foil which can occur at high temperatures in the presence
of oxygen. Once you have verified the ECD’s operation at this temperature, you
may heat it to higher temperatures.
4. Turn on the ECD standing current (the ECD current ON / OFF switch is
located on the front control panel of the GC, under “DETECTOR
ECD standing current
PARAMETERS”). As a rule of thumb, an ECD detector requires enough nitrogen ON/OFF switch
makeup flow (40-100mL/min) to significantly dilute the carrier in order to help
keep detector noise down; the ECD can tolerate a 6:1 ratio of nitrogen to helium.
With the carrier and makeup gas connected and flowing, check the
offset from zero. The millivolt reading should be between 100 and
500mV. If the signal offset is less than 100mV, the standing current
needs to be increased. If the signal offset is higher than 500mV, the
standing current needs to be decreased. Once the signal is relatively
quiet and stable, set the temperature to whatever is appropriate for
your analysis by adjusting the trimpot setpoint with the flat blade
screwdriver provided.
5. When the ECD detector cell reaches temperature, let the system
ECD cell temperature display
stand until you get a stable milliVolt reading. Once the system exhibits
a stable baseline, reconnect the column. Observe the signal in the
presence of the carrier flow. If it is significantly higher, it indicates
contamination introduced on the carrier flow. If the milliVolt reading is still relatively stable in the presence of
carrier flow, then sample may be injected. Avoid samples with high concentrations of electronegative
compounds; they may effect ECD operation for some time thereafter, as they could take too long to dissipate.
6. You may need to adjust the ECD standing current using its trimpot setpoint. The trimpot setpoints are
located on the top edge of the front control panel, directly above the display push-buttons for each controlled
zone. Remember, increasing the standing current increases the ECD’s sensitivity and raises the baseline offset.
 DETECTORS
Electron Capture Detector - ECD

ECD Troubleshooting

If you are experiencing baseline offset and noise problems withyour ECD detector, try the following two
diagnostic tests:

1. Verify that the ECD amplifier electronics are working properly by removing the detector from the circuit and
inserting a 1000MOhm test resistor in its place. The parts kit in the tackle box included with your GC under
the red lid contains a 1000MOhm resistor for this test. Turn the ECD current off. The anode and cathode
connections are BNC connectors located on the GC chassis near the base of the ECD detector housing.
Disconnect these two BNC connectors from the detector electronics, and install the 1000MOhm test resistor
as a jumper between the center conductor in the anode BNC jack and the center conductor in the cathode
BNC jack. Zero the data system signal. Turn the ECD current back on, and check the signal offset (observe
the mV reading in the upper right area of the PeakSimple chromatogram window. With the test resistor in the
detector’s place, the signal offset should be 120-150mV with the standing current at 300. If the signal offset
is pegged up or down (5000mV or 1500mV, respectively), there is a problem with your ECD detector
electronics. Try turning off the GC power for at least 30 seconds, with the test resistor still in place, then turning
it back on to see if the signal offset still indicates a problem. If the signal offset is at zero with the test resistor
in place, check to make sure that you are looking at the correct detector channel. If you are observing a signal
offset of zero in the ECD detector channel, call technical support.

The ECD anode and cathode

are connected to the ECD
Anode and cathode ECD electronics test
amplifier via BNC cables
BNC connectors

BNC cables from ECD

Test resistor

1000MΩ

Anode Cathode

2. Operate the ECD on make-up gas only by disconnecting the column from the ECD. With the standing
current still set at 300, observe the signal offset and noise. If it drops, then the problem is being introduced into
the GC and ECD by the carrier gas through the column.

Tip: In most situations, the ECD will be used to detect sample components that are reactive with metal. Use
glass, fused silica, or fused silica lined metal capillary columns to help avoid reactive sites and ghost peaks.