DETECTORS

Flame Photometric Detector - FPD

Overview

The Flame Photometric Detector is similar to the FID in that the

sample exits the analytical column into a hydrogen diffusion flame.
Where the FID measures ions produced by organic compounds
during combustion, the FPD analyzes the spectrum of light emitted
by the compounds as they luminesce in the flame. The detector FPD/FID
chamber must be light tight so that only light from the flame will be detector
“seen” by the photomultiplier tube (PMT) and analyzed. The FPD
uses a second hydrogen flow to purge the optical path between the
PMT and the hydrogen diffusion flame. This second hydrogen flow
helps to augment the FPD sensitivity by making
the flame hydrogen rich. The FPD also uses a
FPD detector equipped with an FID collector
second air flow directed across of the face of
the PMT to prevent helium and/or hydrogen FID collector Exhaust
molecules from permeating the PMT’s glass electrode tube
window and causing malfunction. This purge Ignitor
air is vented to atmosphere through a short tube,
PMT
coiled to prevent light from reaching the PMT. housing
The FPD uses one of two available band pass air purge Bandpass
filters to selectively detect compounds outlet filter and
PMT
containing sulfur or phosphorus. Compounds
containing phosphorus are detectable with the
526nm filter, which is yellow on one side. The
394nm filter (blue on one side) allows detection
of sulfur-containing compounds. While not
completely selective, the FPD is 100,000 times
Hydrogen &
more sensitive to sulfurous and phosphorous air supplies
compounds than it is to hydrocarbons. Sulfur
compounds like H2S or SO2 can be detected
down to about 200ppb; phosphorus Exhaust
cap nut
compounds can be detected down to 10ppb. To detect
phosphorus and sulfur at the same time, the Dual FPD,
featuring two PMTs, may be used. The single or dual FPD
may be equipped with an FID collector electrode and
electrometer which will detect the hydrocarbon peaks as
the PMTs are responding to the sulfur and phophorus
compounds. Because the hydrogen-rich flame required for
optimum sulfur and phosphorus detection is not optimum
for the best hydrocarbon response, the FID in combination FID collector
with the FPD is less sensitive than a pure FID response. electrode
DETECTORS
Flame Photometric Detector - FPD

Theory of Operation

The FPD uses one of two available band pass filters over a photomultiplier tube (PMT) to selectively
detect compounds containing sulfur or phosphorus as they combust in the hydrogen flame. When compounds
are burned in the FPD flame, they emit photons of distinct wavelengths. Only those photons that are within the
frequency range of the filter specifications can pass through the filter to the PMT. The PMT converts the
photons it “sees” through the bandpass filter to an analog signal, which is acquired by the Peak Simple data
system.

Simplified FPD Schematic

Exhaust tube

Jet Ignitor blade

Ignitor
Column
effluent
Photons

Ferrule
Air
inlet
Primary H2 Bandpass filter over
inlet to jet PMT window (394nm
for sulfur, 526nm for
Secondary H2 inlet H2 phosphorus)
into PMT housing
Purge air inlet Purge air outlet

Stainless steel
retaining nut Photomultiplier
Rubber o-ring tube (PMT)

Photomultiplier signal
Split TeflonTM ferrule
cable to amplifier
10-pin socket
 DETECTORS
Flame Photometric Detector - FPD

Expected Performance

FPD Noise Run (FID/FPD Combo)

Column: 15m MXT-1

Carrier: Helium @ 10mL/min
FPD gain: HIGH
FPD temp: 150oC
FPD PMT volts: -400
FPD noise averages less than 100µV
FPD H2: 60mL/min (30mL/min for each of
from peak to peak
the two hydrogen flows)
FPD air: 100mL/min

FPD Sulfur (FID/FPD Combo)

Sample: 1cc 10ppm H2S in 3 replicate
injections to demonstrate the
consistency of the FPD response
Column: 15m MXT-1
Carrier: Helium @ 10mL/min
FPD gain: HIGH; FPD temp: 150oC
FPD PMT volts: -400
FPD H2: 60mL/min (30mL/min for each of the
two hydrogen flows)
FPD air: 100mL/min
Temperature Program:
Initial Hold Ramp Final
60 oC 60.00 0.00 60 oC
Results:
Component Retention Area
Hydrogen Sulfide 6.550 5216.6680
Hydrogen Sulfide 7.533 4828.8710
Hydrogen Sulfide 8.516 4810.5420
Total 14856.0810
FPD Phosphorus
Sample: 1µL 10ppm malathion
Column: 15m MXT-1
Carrier: helium @ 10mL/min
FPD PMT volts: -400
FPD H2: 30mL/min
FPD air: 100mL/min
FPD temp: 250oC

Temperature Program:
Initial Hold Ramp Final
225oC 10.00 0.00 225oC

Results:
Component Retention Area
Malathion 4.916 2819.0520
DETECTORS
Flame Photometric Detector - FPD

General Operating Procedure

1. Set the hydrogen flow to 60mL/min. This correlates to a flow of 30mL/min each for the primary and
secondary hydrogen. Set the air supply to 100mL/min. The air supply tubing is T’d inside the GC so that 10-
30mL/min of air flows across the face of the PMT. Set the carrier gas flow between 5 and 20mL/min.
2. Use the switch on the GC’s front control panel to light the FPD flame. Sometimes the flame is difficult to
light because of the hydrogen-rich atmosphere inside the FPD detector body. If you are having difficulty
lighting it, make sure the PMT voltage is OFF, then remove the cap on the FPD exhaust port and try the ignitor
switch again. When the flame lights, there will be a loud noise like the backfiring of a car; this is normal and
does not indicate a problem. KEEP YOUR FACE AWAY FROM THE DETECTOR WHILE LIGHTING
THE FLAME; the loud noise is accompanied by a flash of flame. Replace the exhaust cap nut after lighting the
flame.
3. Switch on the PMT voltage and set it to 400 by using the provided flat blade screwdriver to adjust the
trimpot setpoint on the top edge of the GC’s front control panel (vertically labeled “PMT VOLTS” under
“DETECTOR PARAMETERS”).
4. Set the FPD temperature to 150oC by adjusting the appropriate trimpot setpoint. Set the FPD gain to
HIGH. Allow the FPD signal to stabilize, then inject the sample.

Optimizing Sensitivity

To optimize your FPD detector’s sensitivity, inject the same sample at varying air and hydrogen pressures
and observe the fluctuations in sensitivity.
1. Inject sample and observe the FPD response.
2. Turn the air up a tiny bit, less than 1psi, inject sample and observe the FPD response again. If you see an
improvement in sensitivity, adjust the air up a little more, inject again and observe the response. Keep adjusting
the air pressure up until sensitivity drops again to find the window of optimum sensitivity.
3. If there is no improvement in sensitivity after turning the air up, turn the air down less than 1psi, inject
sample and observe the FPD response. If you see an improvement in sensitivity, adjust the air down a little
more, inject again and observe the response. Keep adjusting the air pressure down until sensitivity drops again
to find the window of optimum sensitivity.
4. Now, turn the hydrogen pressure up 1-2psi and re-optimize the air. Repeat this until you’ve found the
optimum air and hydrogen pressure settings.

Note:
When a large hydrocarbon peak elutes simultaneously with a target sulfur compound, the hydrocarbon
peak will quench the sulfur response. For this reason, SRI recommends the addition of an FID collector
electrode to the FPD detector body. The FID collector electrode will allow the operator to “see” the hydrocarbon
peaks and their retention times, so that chromatographic separation can be optimized for the elution of sulfur
compounds.
 DETECTORS
Flame Photometric Detector - FPD

Switching Between Sulfur and Phophorus Modes

The bandpass filter specified when the instrument was ordered comes installed in the FPD detector assembly.
There are two options for switching between sulfur and phophorus modes. You can purchase either an
additional filter or an additional PMT housing and switch them as necessary. Phosphorus wavelength filters are
available under SRI part number 8670-0083; sulfur filters are available under SRI part number 8670-0082. A
PMT housing with a bandpass filter of the other optional wavelength specifications is available under SRI part
number 8670-0084 (specify sulfur or phosphorus).
1. Turn OFF the GC power.
2. Unplug the BNC cable connecting the PMT to the amplifier. Loosen
Disconnect the secondary hydrogen and both air supply lines at this fitting
their bulkhead fittings on the GC deck.
3. Remove the heater block cover by unscrewing the philips
head screw on top of it. Slide the cover up and off the block,
and carefully remove the white insulation.
4. Loosen the 1/8” Swagelok fitting that secures the FPD detector +45
-
o

assembly on the heater block enough to gently rotate the FPD

GC front
assembly about 45o toward the front
Loosen of the GC (see the Front View and Front view Side view
this fitting Side View illustrations to the right).

Slide the PMT 5. Stabilize the FPD assembly while you loosen the 1/4” Swagelok fitting that
housing out secures the PMT housing to the FPD detector body. Slide the PMT housing out
of the FPD
of the detector body. If you’re switching PMT housing assemblies, set aside the
body
PMT housing you just removed and skip to step number 7. If you’re switching
filters, proceed to the next step.
6. Unscrew the PMT housing stainless steel Use these
retaining nut, then set it (with the PMT and its depressions
socket) aside. The bandpass filter is screwed for filter removal

into the top part of the PMT housing against a

black o-ring, and has 2 depressions in its frame. It can be unscrewed using
open needle-nosed pliers but you must be very careful not to damage or Filter inside PMT
housing assembly
scratch the filter. FPD sensitivity will be reduced if the filter is improperly
installed or dirty.
6. Inspect the black o-ring for any nicks or cuts and replace it if necessary. Place the alternate filter, with its
colored side facing down toward the PMT, into the top part of the PMT housing against the black o-ring and
tighten it. Remember, it must be light-tight and gas-tight. Replace and tighten the stainless steel retaining nut
with the PMT in its socket.
7. Slide the top of the PMT housing containing the alternate filter into the FPD detector body, and tighten the
1/4” fitting that secures it in place.
8. Gently rotate the FPD assembly back to its original angle, and tighten (with a wrench) the 1/8” fitting that
secures it to the heater block. Reconnect the gas supply lines and the BNC cable. See the note on the
following page regarding proper jet positioning.
DETECTORS
Flame Photometric Detector - FPD

Troubleshooting and Maintenance

Changing the Photomultiplier Tube (PMT)
The Photomultiplier Tube (PMT) is a consumable part, and will eventually need replacement.
Additional PMTs are available under SRI part number 8670-0080.
1. Follow steps 1-4 on the “Switching Between Sulfur and Phophorus Modes” page.
2. Unscrew the stainless steel retaining nut and remove it,
with the PMT and its socket, from the FPD assembly. Slide
the retaining nut down the PMT amplifier lead to access PMT Housing
the PMT. Assembly
3. Unplug the PMT from its socket. Remove the split
TeflonTM ferrule and black o-ring from the PMT, inspect Black o-ring
them for any damage, and replace them if necessary.
4. Slide the TeflonTM ferrule and black o-ring onto the new Bandpass
PMT. Plug the new PMT into the socket. filter
5. Slide the stainless steel retaining nut up and around the
Photomultiplier Black o-ring
PMT, and screw it into place.
Tube (PMT)
6. Gently rotate the FPD assembly back to its original Split TeflonTM
angle, and hand tighten the 1/4” fitting that secures it. ferrule

7. Reconnect the BNC cable and the gas supply lines. 10-pin socket

Note: When your FPD detector was assembled at the

factory, the ignitor and jet (and collector electrode, if
present) were all properly positioned within the FPD body. Top view of FPD with exhaust cap nut removed
It is advisable to familiarize yourself with their proper
positioning in case they require adjustment. Remove the
1/4” Swagelok cap nut on the FPD exhaust port to see
inside the detector body. Use a small flashlight to see the Use this 1/4” fitting Ignitor fitting
position of the jet inside the FPD detector body. The jet’s to adjust the
tip should be flush with the cylindrical wall of the opening position of the jet
that you’re looking through, and just barely visible from a Collector
slight angle. When looking straight down into the opening, fitting
you should not be able to see anything protruding into it.
To adjust the jet, loosen or tighten the 1/4” Swagelok fitting
to move the jet forward or backward. Keep in mind that
if the jet actually protrudes into the PMT’s line of sight, it An angled view reveals the tip of the jet
could interfere with the FPD’s performance. The ignitor
should be similarly positioned across from the jet, with the
tip of its blade just visible but not protruding into the FPD
detector body chamber. To adjust the position of the ignitor,
loosen the 1/4” fitting enough to move the ignitor forward
or backward as necessary. Tighten the fitting when the
ignitor is properly positioned. If there is an FID collector
electrode installed on the FPD detector assembly, it must
be positioned in the same manner.