6890_Single_and_Dual_FPD

Agilent G2333B (Single)
and G2334B (Dual)
Flame Photometric
Detectors
For Agilent 6890 GC
Installation and Operation
Agilent Technologies
Notices
© Agilent Technologies, Inc .2004, 2005
Warranty
No part of this manual may be reproduced in
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into a foreign language) without prior agreement and written consent from Agilent
Technologies, Inc. as governed by United
States and international copyright laws.
The material contained in this document is provided “as is,” and is subject to being changed, without notice,
in future editions. Further, to the maximum extent permitted by applicable
law, Agilent disclaims all warranties,
either express or implied, with regard
to this manual and any information
contained herein, including but not
limited to the implied warranties of
merchantability and fitness for a particular purpose. Agilent shall not be
liable for errors or for incidental or
consequential damages in connection with the furnishing, use, or performance of this document or of any
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terms, the warranty terms in the separate agreement shall control.
Manual Part Number
G1535-90328
Edition
Fourth edition, May 2005
Third edition, April 2005
Second edition, August 2001
First edition, May 2000
Printed in USA
Agilent Technologies, Inc.
2850 Centerville Road
Wilmington, DE 19808-1610 USA
Acknowledgements
Torx® is a U.S. registered trademark of
Textron, Inc.
2
Safety Notices
CAUTION
A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like
that, if not correctly performed or
adhered to, could result in damage
to the product or loss of important
data. Do not proceed beyond a
CAUTION notice until the indicated
conditions are fully understood and
met.
WA R N I N G
A WARNING notice denotes a
hazard. It calls attention to an
operating procedure, practice, or
the like that, if not correctly performed or adhered to, could result
in personal injury or death. Do not
proceed beyond a WARNING
notice until the indicated conditions are fully understood and
met.
FPD Installation and Operation
Contents
1
Installation
Kit Contents
9
Required Tools
11
Introduction 12
Single-wavelength FPD 12
Dual-wavelength FPD 12
Detector construction 12
Typical Installation
Overview
15
16
Prepare the GC
17
Remove the Covers and Panels
Prepare the Detector Location
Install the Flow Module
18
19
21
Install the Detector 24
Detector body 24
Heater/Sensor cables 25
Signal boards 28
Signal board cable connections
29
Update the Firmware 31
6890A and 6890 Plus 31
6890N 32
Replace the Covers and Panels
33
Return the GC to Operating Condition
FPD Installation and Operation
34
3
2
Checkout Procedure
Overview 36
Materials needed
36
Creating Methods 38
Phosphorus method 38
Sulfur method 40
Using ChemStation macros
Running the Tests
41
42
Interpreting Results 46
For phosphorus 46
For sulfur 46
3
Operation
General Rules 48
Starting up 48
Shutting down 48
Photomultiplier (PMT) protection
Lit Offset 48
High-purity gases 48
Installing Columns 50
Capillary columns 50
Packed columns, 1/8-inch
Packed columns, 1/4-inch
4
48
51
52
Maintenance and Troubleshooting
Changing the Wavelength Filter
Accessing Heaters and Ignitor
54
58
Replacing the Heater/Sensor Assemblies
Replacing the Ignitor
4
62
69
FPD Installation and Operation
Replacing the Inert Transfer Line 73
Removing the transfer line 73
Reassembly 75
Troubleshooting 76
Offset or detector output too high or too low 76
MDL too high 76
High noise level 77
Small peak area 77
Large peak width at half-height 78
Detector Temperature Not Ready (6890) 78
Clipped peaks 79
Data lost because detector tries to reignite during a run
Flame extinguishes after ignition 80
A
80
Replacement Parts
Inert Transfer Line
84
FPD Ignitor and Heat Shield Assembly
FPD Lens Assembly
88
PMT and Bracket Assemblies
90
Covers, Flow Modules, and Electronics
FPD Installation and Operation
86
92
5
6
FPD Installation and Operation
Agilent G2333B and G2334B Flame Photometric Detectors
Installation and Operation
1
Installation
Kit Contents 9
Required Tools 11
Introduction 12
Single-wavelength FPD 12
Dual-wavelength FPD 12
Detector construction 12
Typical Installation 15
Overview 16
Prepare the GC 17
Remove the Covers and Panels 18
Prepare the Detector Location 19
Install the Flow Module 21
Install the Detector 24
Update the Firmware 31
Replace the Covers and Panels 33
Return the GC to Operating Condition 34
Agilent Technologies
7
1
Installation
The G2333B and G2334B kits each contain a flame photometric detector
(FPD) for the Agilent 6890 Series gas chromatograph (GC). Table 1 describes
each kit further.
Table 1
8
FPD installation kits
Kit
Description
G2333B
Contains a single-wavelength FPD, which requires you to change the
wavelength filter when switching between sulfur and phosphorus detection
modes.
G2334B
Contains a dual-wavelength FPD, which enables you to collect both sulfur and
phosphorus data at the same time.
FPD Installation and Operation
Installation
1
Kit Contents
Table 2 lists the parts for both kits.
Table 2
Kit contents
Description
Kit 2333B
Single-wavelength
Kit 2334B
Dual-wavelength
• Aux zone/valve box cable
1
1
• Auxiliary heater bracket
1
1
• Screw, M4 × 12 mm, unthreaded shank
2
2
• Electronics pan cover
1
1
• Electronics top cover
1
1
• Ground strap assembly
1
1
FPD assembly,
(single detector + flow module + board)
1
Auxiliary heater assembly, consisting of:
Electronics cover, consisting of:
FPD assembly,
(dual detector + flow module + board)
1
Screw, M4 × 12 mm, threaded shank
5
5
Cable tie
1
1
Hex nut, M4
1
1
Hex nut, 5/16-inch
3
3
ROM set Revision A.03.08
1
1
HOT label warning
1
1
Detector top cover
1
1
Back top panel
1
1
1
1
Shipping kit, containing:
• Silicone tubing, 30-inch
FPD Installation and Operation
9
1
Installation
Table 2
CAUTION
10
Kit contents (continued)
Description
Kit 2333B
Single-wavelength
Kit 2334B
Dual-wavelength
• Phosphorus filter
1
1
• Column nut
1
1
• Column tool
1
1
• Ferrule, 1/8-inch, 15% graphite, 85% Vespel
1
1
• Ferrule, No-hole
1
1
• Capillary adapter seat
1
1
• Capillary adapter nut
1
1
• Nut, 1/8-inch, stainless steel
1
1
• Packed column adapter
1
1
• Wrench, 3/8-inch × 7 mm
1
1
It is neither necessary nor advisable to separate detectors from their flow modules. Doing
so can create leaks. Although handling the detector and flow module as a unit is awkward,
it can be managed.
FPD Installation and Operation
Installation
1
Required Tools
• T-20 Torx® screwdriver
• Knife
• Chip removal tool (Amp 821903-1 or equivalent)
• Column measuring tool (for capillary columns)
• Isooctane
• Column cutter
• Grounded wrist strap
• Clean, lint-free gloves
• Cotton swabs on wooden sticks
• Lint-free cloth
• Diagonal cutters
• 1/4-inch open-end wrench
FPD Installation and Operation
11
1
Installation
Introduction
The column effluent is burned in a hydrogen-rich flame. The excited species
decay in the cooler region above the flame and emit light. This is viewed by a
factory-calibrated photomultiplier tube (PMT). A shield blocks light from the
flame itself, while filters isolate the light from sulfur or phosphorus species.
Single-wavelength FPD
You can install one or two single-wavelength FPDs. If you install only one,
place it in the back location.
Each single-wavelength FPD has a signal board that mounts in a slot on the
right side of the GC. The board for the front detector must be in the front slot;
the board for the back detector must be in the back slot.
The signal, high voltage, and ignitor cables from the detector connect to its
signal board. The heater/sensor cables (two per detector; one short and one
long) plug into connectors on the right side of the GC. Details appear later in
this document.
The flow module mounts in the pneumatics chassis at the back-top part of the
GC. There are specific module locations for the front and back detector
locations, which appear later in this document.
Dual-wavelength FPD
A dual-wavelength FPD has one emissions block assembly and two PMT
assemblies. It must be mounted in the back location. It uses two signal boards,
one in each slot. The ignitor cable must connect to the board in the back slot. It
does not matter which board serves which PMT, but the high voltage and
signal cables for a given PMT must go to the same board. The heater/sensor
cables go to the positions for a back detector. Details appear later in this
document.
The flow module goes in the back detector position.
Detector construction
The FPD consists of a detector body, either single or dual, and one or two PMT
assemblies. See Figure 1.
12
FPD Installation and Operation
Installation
1
Body
Dual FPD, exploded view
PMT assembly
PMT assembly
Single FPD, body only, assembled
Figure 1
Single and dual FPD
Most of the illustrations in this document show the single-wavelength body.
Parts are identified in Appendix A.
FPD Installation and Operation
13
1
Installation
Detector body
The detector body consists of:
• A base that mounts to the GC
• A transfer line that conducts the column effluent to the emissions block
assembly
• A sheet metal chimney that encloses the transfer line
• An emissions block assembly with one (single-wavelength) or two
(dual-wavelength) windows and one or two support brackets for PMT
assemblies
• One or two lens and filter holders that mount over the emission block
windows and connect to the PMT assemblies
• A vent tube to remove gases from the detector and prevent room light from
entering the emissions block assembly
PMT assembly
A PMT assembly consists of:
• A long tube to place the temperature-sensitive photomultiplier tube well
away from the heated emissions block assembly
• An end cap that contains the photomultiplier tube and socket
14
FPD Installation and Operation
Installation
1
Typical Installation
Figure 2 shows the parts for a single-wavelength FPD mounted in the back
location. For the front location, the flow module goes in the slot to the right
(when facing the back of the GC) of the one shown and the detector and board
are moved to the front location and slot.
FPD
Detector flow
module
Electronics
pan cover
Hot warning
label
Electronics top cover
Auxiliary heater
bracket and harness
(shown assembled)
Signal board
(1 or 2)
Figure 2
A typical single-wavelength installation
A dual FPD will have two of the long photomultiplier assemblies and mount in
the back location. There will be two signal boards.
FPD Installation and Operation
15
1
Installation
Overview
CAUTION
Perform this installation only if you are experienced in GC maintenance. If not, trained
Agilent personnel can install the FPD.
1 Check the contents of the kit with those listed on page 9.
2 Prepare the GC.
3 Remove the covers and panels.
4 Prepare the detector location.
5 Install the flow module.
6 Install the detector.
7 Update the firmware, if applicable.
8 Replace the covers and panels.
9 Change the wavelength filter, if necessary.
10 Return the GC to operating condition.
11 Test the FPD (see Chapter 2, “Checkout Procedure” for more information).
16
FPD Installation and Operation
Installation
1
Prepare the GC
1 Turn off the GC and unplug the power cord.
WA R N I N G
Hazardous voltages are present in the instrument whenever the power cord is
connected. Avoid a potentially dangerous shock hazard by disconnecting the power
cord before working on the instrument.
WA R N I N G
Hydrogen gas is flammable and potentially explosive. Before installing the detector,
turn off the hydrogen gas at the source.
2 Turn off all gas supplies.
3 Remove columns and hardware associated with both detectors from the
oven to clear the way for the FPD.
FPD Installation and Operation
17
1
Installation
Remove the Covers and Panels
You must remove several covers of the GC. Figure 3 shows a suggested order of
removal.
4. Pneumatics chassis cover
Lift up on each end to release the
clips and remove the cover.
1. Top cover
Raise to the vertical position. Raise the
right side and remove it. Discard the cover.
3. Electronics cover
Reach under the cover, release the
clips, and lift the cover. Discard the
cover.
6. Back-top panel
Remove the three screws.
5. RFI cover
Remove the screw, and slide the plate
to the left to disengage the tabs.
2. Right-side panel
Loosen the two captive screws
along the top edge. Slide the
panel toward the back. At the top,
tilt outward, and lift.
Figure 3
18
Removing covers and panels of the 6890 GC
FPD Installation and Operation
1
Installation
Prepare the Detector Location
CAUTION
It is neither necessary nor advisable to separate detectors from their flow modules.
Doing so can create leaks. Although handling the detector and flow module as a unit is
awkward, it can be managed.
1 Select the location—front or back—where you will install the FPD. If
possible, install it in the back position.
WA R N I N G
To avoid damaging the printed circuit board electronics, use a grounded wrist strap
(part number 9300-1408) and connect it to a bare metal surface of the GC.
2 If a detector is presently mounted in the selected location, remove it and its
flow module. Flow modules are held by a single screw from the front.
Remove the screw and slide the module, the detector, and other
attachments out the back of the chassis. See the GC user information for
details.
If the current detector is to be installed in the other detector location, see
that detector’s documentation for details.
3 Install the hot warning label above the oven door. See Figure 2 on page 15.
Align it with the left edge of the large hole and the back edge of the blue bar.
WA R N I N G
The insulation on the GC is made of refractory ceramic fibers. Ventilate your work
area. Wear long sleeves, gloves, safety glasses, and a disposable dust/mist
respirator. Dispose of insulation in a sealed plastic bag.
If the detector location has not been used before
1 The detector location may be covered by a metal knockout plate. Either cut
the webs that hold it or use a screwdriver in the center slot to bend it back
and forth until the webs break. Discard the plate.
FPD Installation and Operation
19
1
Installation
2 There are two layers of insulation on top of the oven. Use a sharp knife to
cut through the top layer—the soft one—using the hole in the metal as a
template. Remove the soft insulation to expose the hard insulation.
3 The hard insulation has a precut hole that is filled with a plug. Push the
plug out into the oven and discard it
If the location has been used before
1 Remove any insulation left over from a previous detector. Check that the
hole in the soft insulation conforms to the hole in the metal top plate.
2 If the precut hole in the hard insulation is still plugged, push the plug out
and discard it.
20
FPD Installation and Operation
Installation
1
Install the Flow Module
CAUTION
It is neither necessary nor advisable to separate detectors from their flow modules. Doing
so can create leaks. Although handling the detector and flow module as a unit is awkward,
it can be managed.
1 The tubing between the detector and flow module has been folded for
shipping. Unfold the tubing, being very careful to avoid kinks or tight bends.
2 Locate the correct slot for the flow module (Figure 6).
• If the detector is to be mounted in the back location, use the second slot
from the left (as viewed from the back of the GC). Note that a
dual-wavelength detector must be mounted in the back location.
• If the detector is to be mounted in the front location, use the third slot
from the left (as viewed from the back of the GC).
CAUTION
Hold the flow module by its support bracket to avoid damaging the components.
3 Route the ribbon cable behind the flow module assembly as shown in
Figure 4. Then slide the flow module and bracket assembly into the slot
until the bracket seats flush against the end of the rails (see Figure 5).
Back of
flow module
Ribbon cable
Figure 4
FPD Installation and Operation
Ribbon cable goes behind the flow module
21
1
Installation
Tubing to detector
Bracket flush
with rail
Figure 5
Flow module installed
4 Connect the ribbon cable to the mating connector on the pneumatics board.
The mating connector for the flow module is not the one directly under it.
The connectors are identified by raised lettering on the plastic immediately
above them.
Arrange the cable to keep it away from the valves on the right side and keep
it from being pinched against the flow module.
22
FPD Installation and Operation
Installation
1
For the back detector, you may want to loosen the flow module and slide it
out of the carrier a few centimeters to connect the cable to the pneumatics
board. Then, reinstall the flow module.
a Secure the flow module in place using the T-20 Torx mounting screw on
the front of the pneumatics chassis.
b Use a pair of diagonal cutting pliers to remove the appropriate back-top
panel cutout. Also remove any cutouts needed to access other flow
modules or accessories installed in the GC. See Figure 6.
Insert tip of
pliers here
Front detector
Back detector
Figure 6
FPD Installation and Operation
Back-top panel cutouts
23
1
Installation
Install the Detector
CAUTION
It is neither necessary nor advisable to separate detectors from their flow modules. Doing
so can create leaks. Although handling the detector and flow module as a unit is awkward,
it can be managed.
Detector body
1 Cut the shipping tie-wrap holding the PMT assembly to the bracket. Be
careful not to cut any wires. See Figure 7.
CAUTION
There are two tie-wraps. One is the cable tie-wrap that you do not want to cut.
2 The detector body has an extended bottom plate on one side. Place the
detector in the selected location with the extended plate to the right and
with the column fitting passing through the insulation into the oven.
3 The detector is held to the oven top by four screws, one at each corner.
Insert the two screws on the right but do not tighten them (see Figure 7).
DO NOT CUT THIS CABLE TIE-WRAP!
Cut and remove
PMT assembly
Chimney back cover
Left side screws
(one concealed)
Right side screws
Bottom plate
Figure 7
24
Installing the detector (cables removed for clarity)
FPD Installation and Operation
1
Installation
4 Install the two screws on the left side through the chimney cover and the
detector base. Press the cover against the detector and tighten the screws.
5 Tighten the screws on the right side.
6 Bend the gas lines from the flow module downward to one of the T-slots in
the bracket on top of the oven. Pass the lines through the slot. Form excess
length into an S-curve on top of the oven.
7 The FPD produces considerable water vapor when the flame is on. Connect
the silicone tubing from the kit to the curved vent tube on top of the
detector. Run the other end to a suitable container or drain.
Heater/Sensor cables
CAUTION
The next steps require precautions against electrostatic discharge. Use the grounded
wrist strap (part number 9300-1408) and connect it to a bare metal surface of the GC.
Failure to heed this caution may result in damage to the instrument or to the printed
circuit board.
There are two heater/sensor cables for each detector; one for the emissions
block assembly and one for the transfer line. Both cables have woven glass
sleeves but one is much longer than the other.
Short heater/sensor cable
The short heater/sensor cable plugs into a connector on the right side of the
GC, as shown in Figure 8. There is only one way that the connectors will go
together.
FPD Installation and Operation
25
1
Installation
Connector for back detector
Connector for front detector
Figure 8
Short heater/sensor cable connectors
Long heater/sensor cable
To connect the long heater/sensor cable:
1 Locate connector P22 on the GC main board (see the arrow in Figure 9).
Figure 9
26
Long heater/sensor cable connector
FPD Installation and Operation
1
Installation
2 If this connector has a wiring harness and bracket attached to it (see
Figure 10), skip to step 7. If nothing is attached to the connector, continue
with step 3.
Auxiliary heater
bracket
Wiring harness
P22 connector on main board
Figure 10
Wiring harness and bracket
3 Push the wiring harness ends into the auxiliary heater bracket from the
bottom as shown in Figure 11. The connectors are labeled.
A1 connector
A2 connector
Tighten two screws
Plug into 2 × 8 connector
Figure 11
Attaching the assembly to the GC
FPD Installation and Operation
27
1
Installation
4 Plug the large connector on the wiring harness into the P22 connector on
the main board (see Figure 9 and Figure 11).
5 Install the screws with the unthreaded shank into the bracket. The screws
will become captured by the bracket.
6 Attach the bracket to the GC frame.
7 Pass the long heater/sensor cable under the board and plug it into a
connector (see Figure 10) on the bracket as listed in Table 3.
Table 3
Long heater/sensor cable connectors
Detector type
Location
Connector
Single-wavelength
Front
A1
Single-wavelength
Back
A2
Dual-wavelength
Back
A2
Signal boards
1 Install the detector signal board(s) on the right side of the instrument
behind the keyboard (see Figure 12).
Connector, bracket
on other side
Guide for back detector board
Guide for front detector board
Figure 12
28
Installing the detector board(s)
FPD Installation and Operation
1
Installation
2 Insert the board in the correct guide for the location used.
• For a single-wavelength detector, the board goes in the guide for the
detector position used.
• For a dual-wavelength detector, boards go in both guides. The board in
the back slot becomes the master board, providing high voltage and
signal processing for one PMT assembly and ignitor power for the
detector emissions block assembly. It controls the other board.
• The board in the front guide provides high voltage and signal processing
for the second PMT assembly.
3 Press the board firmly into place so that the connector on the board
engages the matching connector on the GC main circuit board.
4 Secure the board with the captive screw in the bracket.
Signal board cable connections
CAUTION
With a dual-wavelength FPD, it does not matter which of the two circuit boards is used
for which PMT (see Figure 12). However, the high voltage and signal cables from each
PMT must go to the same board. Do not “cross-wire.”
1 Connect the cables to the signal boards. Collect the cables and route them
through the metal clip on the side of the PMT assembly support.
Figure 13 locates the detector board connectors.
High-voltage connector
Signal connector
Plugs into main board
Ignitor connector
Figure 13
FPD Installation and Operation
Detector board connector locations
29
1
Installation
High voltage cable
The high voltage cable is black with a chrome connector on the end
(Figure 14). Press it down over the high voltage connector on the board
until it clicks into place.
Figure 14
High voltage cable
Signal cable
The signal cable is black with a BNC connector on the end (Figure 15).
Press it onto the signal connector on the board and turn the knurled ring to
lock it in place.
Figure 15
Signal cable
Ignitor cable
The ignitor cable is gray and ends in a 2-pin flat connector (Figure 16).
Press it into the ignitor connector on the board until it locks into place.
There is only one way that it can be connected.
If you are installing a dual-wavelength detector, there will be only one
ignitor cable. Connect it to the board in the back detector slot.
Figure 16
30
Ignitor connector
FPD Installation and Operation
Installation
1
Update the Firmware
6890A and 6890 Plus
If the present firmware is earlier than A.03.08, you must replace the chips
with those included in the kit. These chips contain firmware version A.03.08.
NOTE
The GC displays the current firmware version when you first turn it on or press [STATUS]
followed by [Clear].
To replace the chips:
1 Examine the right side of the GC. On the main board, just below the large
cutout on the left, are four chip sockets (see Figure 17). The two on the left
contain the operating programs (firmware) that run the GC.
Chip
Round dimple
Notches for chip
removal tool
0-chip
1-chip
Figure 17
Chip sockets
The chips that came in the kit are identified by a part number, a version
number, and a suffix of either “.0” or “.1”. They are referred to as the 0-chip
and the 1-chip, respectively.
FPD Installation and Operation
31
1
Installation
CAUTION
This procedure requires precautions against electrostatic discharge. Use a grounded
wrist strap (part number 9300-1408) and connect it to a bare metal surface of the GC.
Failure to heed this caution may result in damage to the instrument.
2 Use a chip removal tool with a gentle rocking/pulling motion to remove a
chip from the socket.
CAUTION
Be sure to note which chip you are removing. You want to be sure to place the correct
replacement chip in the correct socket.
3 Orient the chip so the round dimple is at the right. When the chip is
properly aligned, snap it into place in the socket indicated in Figure 17
using firm pressure.
4 Repeat step 2 and step 3 for the other chip.
6890N
To download the latest 6890N firmware, visit the Agilent Web Site at
www.agilent.com/chem, login or register, and navigate to firmware.
32
FPD Installation and Operation
Installation
1
Replace the Covers and Panels
1 Place the back-top panel on its left-most mounting screw. Use the screw as a
hinge and angle the panel while sliding each ID tag through its cutout in the
panel, working from left to right. When all the tags are through the panel,
finish installing the panel on the GC.
2 Re-install the RFI cover, the pneumatics chassis cover, and the top cover.
3 Re-install the right-side panel. Be sure that the hook at the back-top corner
is engaged.
4 The electronics cover that came in the kit is in two parts (see Figure 18).
Pan
Folded lip
Top cover
Ground strap
Front clip
Figure 18
The electronics cover
a Unscrew the four captive screws and remove the pan.
b Align the base and lower it into place. Two clips secure it.
c Slide the pan—folded lip to the right—under the PMT assemblies).
d Attach the groundstrap under the top cover as shown in Figure 18.
Connect it between one of the pan mounting screws and one of the
screws that secure the detector to the top of the oven.
e Align the other screws with the holes and tighten all four.
FPD Installation and Operation
33
1
Installation
Return the GC to Operating Condition
1 Restore power.
2 Turn off the flame to prevent condensation in the detector.
3 Restore gas flows and pressures and check for leaks. See the GC user
information for leak testing information.
4 Reboot the GC. As it is turning back on, check to see if it detects that it has
an FPD. If not, check these connections:
• Detector card to main board
• Flow module to pneumatics board
• Heater/Sensor connections
• Ignition cable to detector card
• High-voltage cable to detector cards
• Signal cable to detector card
• Correct ROM installed on main board
If you have temperature control for the detector but not flow control, check
the connection between the flow module and the pneumatics board.
34
FPD Installation and Operation
Agilent G2333B and G2334B Flame Photometric Detectors
Installation and Operation
2
Checkout Procedure
Overview 36
Creating Methods 38
Phosphorus method 38
Sulfur method 40
Using ChemStation macros 41
Running the Tests 42
Interpreting Results 46
When you have installed the FPD, you should test it to verify that it works
correctly. This chapter describes a test protocol for running sulfur and
phosphorus samples through the GC and examining the results.
The protocol will differ depending on the equipment you have. This chapter
describes the protocol in terms of a ChemStation, but contains sufficient
information so that the tests can be run with just a strip-chart recorder.
Agilent Technologies
35
2
Checkout Procedure
Overview
NOTE
This procedure assumes that the tester is familiar with the safe operation and maintenance
of the gas chromatography system, including the automatic liquid sampler, GC, and data
handling device.
This is the recommended sequence of steps for running the checkout. Install
the column.
1 Create and save the phosphorus and sulfur methods.
2 Load the phosphorus method, turn off the flame and electrometer.
3 Install the phosphorus filter.
4 Set inlet, oven, and detector to 250 °C to bake out for 15 minutes.
5 Reload the phosphorus method. Monitor signal output. This output
typically runs between 40 and 55 but can be as high as 70.
6 When it levels off, run one sample. Interpret the results (page 46).
7 Turn off the electrometer. Install the sulfur filter and spacer.
8 Load the sulfur method. Monitor signal output. The output typically runs
between 50 and 60 but can be as high as 70.
9 When it levels off, run one sample. Interpret the results (page 46).
Materials needed
• Column: 5% Phenyl Methyl Siloxane Capillary 30.0 m × 0.32 mm × 0.25 µm
(part number 19091J-413).
For Japan only: HP-5MS 30 m × 0.32 mm × 0.50 µm (part number
19091S-113).
• Checkout sample, part number 5188-5953.
For Japan only, part number 5188-5245.
• For cool on-column inlet use: 5-mm septa (part number 5183-4758, 50/pk),
5-μL on-column syringe for 320-µm column (part number 5182-0836), and
needle for 320-µm column (5182-0831).
36
FPD Installation and Operation
Checkout Procedure
2
• For split/splitless inlet use: 11-mm septa (part number 5183-4757 50/pk),
10-µL syringe (part number 5181-1267), or equivalent, and a liner. The liner
can be general purpose (part number 5183-4711) or single-taper
deactivated with (part number 5062-3587) or without (part number
5181-3316) glass wool.
For Japan only: 11-mm septa (part number 5183-4757 50/pk), 10-µL syringe
(part number 5181-1267), or equivalent, and a single-taper liner
deactivated without (part number 5181-3316) glass wool.
• Chromatographic-grade iso-octane for syringe wash solvent.
• Chromatographic-grade 99.9995% purity gas: helium as carrier, nitrogen as
makeup, hydrogen and air.
• 4-mL solvent and waste bottles or equivalent for autoinjector.
• 2-mL sample bottles or equivalent for sample.
FPD Installation and Operation
37
2
Checkout Procedure
Creating Methods
Create the test methods using these steps:
1 Create a phosphorus method (Table 4).
2 Save it using a name that identifies it as the phosphorus method (such as
P_Ckout.m).
3 Make a copy and modify the detector flow parameters in the copy to change
it to a sulfur method (page 40).
4 Save the copy using a distinctive name that identifies it as a sulfur method
(such as S_Ckout.m).
Phosphorus method
Table 4 contains the parameters for the phosphorus method. Give the method
a meaningful name that allows you to distinguish it from the sulfur method.
Table 4
Phosphorus checkout method default parameters value
Parameter/Setting
Sample 5188-5953
Sample 5188-5245
Initial temp, °C
70
70
Initial time, min
0.00 min
0.00 min
Rate 1, °C/min
25.00
10.00
Final temp 1, °C
150
105
Final time 1, min
0
0
Rate 2, °C/min
5
20
Final temp 2, °C
190
190
Oven
Final time 2, min
4
1
Agilent 19091J-413, HP5,
30.0 m × 320 µm × 0.25 µm
Agilent 19091S-113, HP5 MS,
30.0 m × 0.32 mm × 0.50 µm
Mode
Constant pressure
Constant pressure
Pressure
25 psi
25 psi
Temperature, °C
200 (On)
200 (On)
Hydrogen flow
75.0 mL/min (On)
75.0 mL/min (On)
Column
Detector
38
FPD Installation and Operation
Checkout Procedure
Table 4
2
Phosphorus checkout method default parameters value (continued)
Parameter/Setting
Sample 5188-5953
Sample 5188-5245
Air (Oxidizer) flow
100.0 mL/min (On)
100.0 mL/min (On)
Mode
Constant makeup flow OFF
Constant makeup flow OFF
Makeup flow
60.0 mL/min (On)
60.0 mL/min (On)
Makeup gas type
Nitrogen
Nitrogen
Flame
On
On
Lit offset
2.00
2.00
Electrometer
On
On
Data rate
5 Hz
5 Hz
Type
Front or back detector
Front or back detector
Save data
On
On
Signal
Zero
0.0 (Off)
0.0 (Off)
Range
0
0
Fast peaks
Off
Off
Attenuation
0
0
Derive from detector
Derive from detector
Temperature, °C
200 (Split/Splitless inlet, and see
below)
Oven track (Cool On-Column inlet)
250 (Split/Splitless inlet, and see
below)
Oven track (Cool On-Column inlet)
Init pressure
25.00 psi (On)
25.00 psi (On)
Gas saver
Off
Off
Mode
Splitless
Splitless
Total flow
69.5 mL/min
69.5 mL/min
Purge flow to split vent
50 mL/min @ 0.75 min
50 mL/min @ 0.75 min
Column Comp 1
Inlet
Split/Splitless inlet
Injector (if installed)
Sample washes
2
2
Sample pumps
8
8
Injection volume
1.0 µL
1.0 µL
Syringe size
5.0 or 10 µL
5.0 or 10 µL
FPD Installation and Operation
39
2
Checkout Procedure
Table 4
Phosphorus checkout method default parameters value (continued)
Parameter/Setting
Sample 5188-5953
Sample 5188-5245
PreInj Solvent A Washes
0
0
PreInj Solvent B Washes
0
0
PostInj Solvent A Washes
4
4
PostInj Solvent B Washes
4
4
Viscosity delay
OFF
OFF
Plunger speed
Fast
Fast
PreInjection dwell
0.00
0.00
PostInjection dwell
0.00
0.00
part number 5188-5953
part number 5188-5245
1.0 µL
1.0 µL
Sample
Injection volume
Additional settings applicable to Agilent data systems are listed in Table 5.
The settings available are for the GC ChemStation. Other data systems vary.
Table 5
Additional settings for Agilent Data Systems
Parameter/Setting
Value
Report settings
Report style
Short or None
Destination
None
Sulfur method
Make a copy (Save As in ChemStation) of the phosphorus method. Rename the
copy to indicate that it is a sulfur method. Edit it as indicated in Table 6.
Table 6
40
Sulfur method parameters
Parameter
Value
H2 flow
50 mL/min
Air flow
60
FPD Installation and Operation
Checkout Procedure
2
Using ChemStation macros
There are two macros designed for ChemStation that you use to interpret and
analyze the data collected from the sulfur and phosphorus tests. Table 7 lists
the macros. They can be downloaded from www.chem.agilent.com/cag/servsup/
usersoft/files/ChemStation_Macros_Collection.htm. Look for Data Systems, then
Downloads and Utilities.
Table 7
ChemStation macros
Macro name
Description
MEPCK_S.MAC
Japan only: fpds_xls.mac
Processes data collected from sulfur tests.
MEPCK_P.MAC
Japan only: fpdp_xls.mac
Processes data collected from phosphorus tests.
These macros calculate the area counts, MDL, and noise, and print a report to
the printer setup in the ChemStation. The report includes the chromatogram,
the noise plot, and several calculations.
Place the macros in the appropriate subdirectory (Table 8) where
ChemStation can find them.
Table 8
Macro subdirectories
Software rev.
Macro location
Summary result log location
B.01.xx or later
CHEM32\CORE
CHEM32\n*
A.10.xx or earlier
HPCHEM\CORE
HPCHEM\n
* n is the instrument number.
The macro can be set to run automatically as part of the method as a post-run
program, or can be run on a loaded data file from the ChemStation Data
Analysis view.
FPD Installation and Operation
41
2
Checkout Procedure
Running the Tests
After setting the conditions, wait for the baseline to stabilize (about 2 hours)
before running samples.
Figure 19 and Figure 20 show typical online plots for sulfur and phosphorus
tests using the checkout methods described in “Creating Methods” on page 38.
Figure 21 and Figure 22 show the same plots for the Japan-only sample.
Methyl parathion
Isooctane
Figure 19
42
Typical chromatogram for sulfur tests, sample 5188-5953
FPD Installation and Operation
Checkout Procedure
2
Methyl parathion
Isooctane
Figure 20
Typical chromatogram for phosphorus tests, sample 5188-5953
FPD Installation and Operation
43
2
Checkout Procedure
tert-Butyldisulfide
1-Dodecanethiol
Isooctane
Figure 21
44
Typical chromatogram for sulfur tests, sample 5188-5245 (Japan only)
FPD Installation and Operation
Checkout Procedure
2
Tributylphosphate
Isooctane
Figure 22
Typical chromatogram for phosphorus tests, sample 5188-5245 (Japan only)
CAUTION
If you receive a message like the following, check your printer setup and make any
corrections.
... has problems. , with page file:
C:\WINNT\TEMP\~P3D042A.TMP
Initial printing problem, 202.
System resources are low and/or device has problems.
NOTE
Depending on the column length, the sulfur chromatograph may contain a contaminate
peak during the noise measurement. Reprocess the run by loading the signal and typing
macro mepck_s.mac,go,3
in the command line. This starts the noise measurement at 3 minutes instead of the default
3.8 minutes.
FPD Installation and Operation
45
2
Checkout Procedure
Interpreting Results
Compare the reported output against the values listed in Table 9 and Table 10.
Your value should be within the limits listed.
For phosphorus
Table 9
Evaluating checkout runs
FPD P filter
Typical range after 24 hours
Limits at installation
MDL (pg/sec)
0.06 to 0.08
≤0.10
Peak area
19000 to 32000
≥19000
Signal height
5000 to 11000
—
Noise
1.6 to 3.0
≤4
Half-width (min)
0.05 to 0.07
—
Signal offset
34 to 80
≤80
For sulfur
Table 10
46
Evaluating checkout runs
FPD P filter
Typical range after 24 hours
Limits at installation
MDL (pg/s)
3.8 to 5
≤6
Peak area
8000 to 19000
≥8000
Signal height
2500 to 6000
—
Noise
2 to 4
≤5
Half-width (min)
0.06 to 0.08
—
Signal offset
34 to 65
≤70
FPD Installation and Operation
Agilent G2333B and G2334B Flame Photometric Detectors
Installation and Operation
3
Operation
General Rules 48
Installing Columns 50
This chapter describes new or changed operating information (at the time of
this printing) that updates the information found in the 6890 user
documentation. Refer to the GC user information for any topics not covered
here.
Agilent Technologies
47
3
Operation
General Rules
Starting up
The FPD creates a great deal of water vapor when the flame is on. This could
condense in the vent tube on top of the detector and drop onto the flame,
possibly extinguishing it. To avoid this, turn the heaters on, wait 20 minutes
for the vent to heat up, and then ignite the flame. Water vapor will now make it
over the top of the vent tube before condensing.
Shutting down
For similar reasons, extinguish the flame before turning the heaters off.
Photomultiplier (PMT) protection
The PMT is extremely sensitive to light. Always turn the electrometer off
(which turns off the high voltage to the PMT) before removing the PMT
assembly or opening the emissions block assembly. Failing to do this can
destroy the PMT.
Even with the electrometer off, protect the PMT from room light. Cap the
housing when removed, place it end down to exclude light, reduce room light
level before exposing the PMT, and so on. A brief exposure (always with the
electrometer turned off) will not damage it but prolonged exposure will cause
a gradual loss of sensitivity.
Lit Offset
The default Lit Offset is 2.0 pA.
High-purity gases
High-purity gases have a lower sulfur content. Standard purity gases have a
higher sulfur content which impairs sulfur detection in the compound being
studied. Instrument or Chromatographic grades work well.
Agilent recommends using helium carrier, nitrogen makeup gas, and air with
99.9995% purity or better. Use hydrocarbon, oxygen, and moisture traps.
Select traps to remove sulfur compounds from detector air and nitrogen gases.
A helium getter is also recommended.
48
FPD Installation and Operation
Operation
3
Inlet liners
Compounds containing sulfur may adsorb to an inlet liner and degrade the
GC’s performance. Use deactivated, clean liners or a cool on-column inlet,
which injects directly onto the column.
For best results with splitless injection, use liner 5181-3316.
FPD Installation and Operation
49
3
Operation
Installing Columns
Capillary columns
CAUTION
Wear safety glasses while handling, cutting, or installing fused silica capillary columns.
To prevent puncture wounds, use care when handling these columns.
The following procedure ensures that the FPD works efficiently. A special tool
is used to cut the column to the correct length.
Swage the column ferrule
1 Install a column nut and ferrule on the end of the column.
2 Insert the end of the column through the column measuring tool
(19256-80640) so that the end protrudes beyond the tool (Figure 23).
Column nut
Ferrule
Column measuring tool
Score column here
Figure 23
Cutting the column to length
3 Tighten the column nut until it grips the column. Use a pair of wrenches to
tighten it an additional 1/8 to 1/4 turn.
4 Use a wafer cutter at 45° to score the column.
5 Snap off the column end.
6 The column may protrude 1 to 2 mm beyond the end of the tool.
7 Remove the column, nut, and swaged ferrule from the tool.
50
FPD Installation and Operation
Operation
3
Install the column
1 Install the capillary adapter in the detector fitting (Figure 24).
FPD fitting
Capillary adapter
1/8-inch nut
Figure 24
Capillary adapter
2 Carefully thread the swaged column up into the adapter. Finger-tighten the
column nut, then tighten an additional 1/8-turn with a wrench.
Packed columns, 1/8-inch
A Type B 1/8-inch column connects directly to the fitting on the bottom of the
FPD. No adapter is required.
FPD Installation and Operation
51
3
Operation
Packed columns, 1/4-inch
1 Install the adapter in the detector fitting (Figure 25). Place the nut and
ferrule on the adapter, insert the adapter into the FPD fitting, and tighten
the nut.
FPD fitting
1/8-inch ferrule
1/8-inch nut
Adapter
Figure 25
1/4-inch column adapter
2 Connect the 1/4-inch column to the adapter in the usual way. Use Type B
glass columns.
52
FPD Installation and Operation
Agilent G2333B and G2334B Flame Photometric Detectors
Installation and Operation
4
Maintenance and Troubleshooting
Changing the Wavelength Filter 54
Accessing Heaters and Ignitor 58
Replacing the Heater/Sensor Assemblies 62
Replacing the Ignitor 69
Replacing the Inert Transfer Line 73
Troubleshooting 76
This chapter describes maintenance procedures that can be performed by an
FPD user. The troubleshooting section is a guide to frequently found things,
including hardware, software, and operational, that can go wrong with
suggestions on how to correct them.
Agilent Technologies
53
4
Maintenance and Troubleshooting
Changing the Wavelength Filter
Changing the wavelength filter takes about 5 minutes. It requires you to turn
off the electrometer, remove the photomultiplier tube assembly, and change
the filter.
CAUTION
Do not touch the filters with your bare hands. For optimum performance and to avoid
scratches, use lint free gloves for assembling and inserting the filters into the
assembly.
Materials needed
• 1000-1437 Sulfur filter and 19256-20910 filter spacer
• 19256-80010 Phosphorus filter
• 5080-5400 Cotton swabs
• Toothpick or cotton swab
• Lens tissue
• 8650-0030 (large) or 8650-0029 (small) Nylon lint-free gloves
Procedure
1 Turn off the detector electrometer.
54
FPD Installation and Operation
Maintenance and Troubleshooting
4
2 Disconnect the retaining spring that holds the PMT assembly to the bracket.
With a rotating motion, pull the assembly away from the filter housing
(Figure 26).
Figure 26
Removing the PMT assembly
3 To prevent light from damaging the PMT, immediately cap the end or place
it face down (Figure 27).
Figure 27
FPD Installation and Operation
Protecting the PMT
55
4
Maintenance and Troubleshooting
4 Place a clean cloth under the filter housing to catch the filter.
Phosphorus filter: use the sharpened wooden tip of a toothpick or cotton
swab to dislodge the filter from the housing.
Sulfur filter: (Figure 28) use the wooden tip of the cotton swab to remove
the filter spacer. Then remove the filter as above.
Sulfur filter
Filter spacer
Figure 28
Sulfur filter and spacer
5 Use lens tissue to clean the new filter. Install it in the filter housing. If you
are installing a sulfur filter, add the filter spacer.
56
CAUTION
Do not use cleaning fluids. Cleaning fluids will damage lens coatings.
CAUTION
Filters are designed for the light from the flame to pass through in a specific direction.
On the edge of the phosphorus filter, there is a triangle. On the edge of the sulfur filter,
there is an arrow. These should face away from the flame and toward the PMT.
FPD Installation and Operation
Maintenance and Troubleshooting
4
6 Replace the PMT assemblies and secure them with the springs.
7 Restore the operating conditions.
FPD Installation and Operation
57
4
Maintenance and Troubleshooting
Accessing Heaters and Ignitor
Removing the vent and cover and, on the dual-wavelength detector, the left
PMT assembly to access the heaters or ignitor takes about 5 minutes. It
requires you to turn off the GC.
CAUTION
When turning the GC off, turn off the flame first to prevent condensation from dripping
into the jet and column.
You may wish to access this area for the following reasons:
• Replace the ignitor.
• Replace seals and O-rings.
• Replace the transfer line assembly.
• Replace or check the heater and PRT sensors.
Materials needed
• 8710-0803 9/16-inch wrench
• 8710-1807 T-20 Torx driver
Procedure
To remove the vent tube and cover
1 Turn off the flame.
2 Turn off the GC.
3 Wait until the detector cools.
58
FPD Installation and Operation
Maintenance and Troubleshooting
4
4 Use a wrench to loosen and remove the vent tube assembly (Figure 29).
Figure 29
Removing the vent tube
5 Single-wavelength detector. Use a Torx T-20 driver to remove the screws
securing the FPD cover. There are two screws at the bottom of the left side
(Figure 30) and two screws at the top of the right side (Figure 31).
Dual-wavelength detector. Use a Torx T-20 driver to remove the screws
securing the FPD cover. There are two screws at the top of the right side
(Figure 31).
Lift the cover off the detector.
FPD Installation and Operation
59
4
Maintenance and Troubleshooting
Figure 30
Cover screws, left side (single-wavelength FPD)
Figure 31
Cover screws, right side (both FPDs)
6 Dual-wavelength detector only. Remove the four screws securing the Dual
FPD chimney front (with the attached dual main bracket and PMT
60
FPD Installation and Operation
Maintenance and Troubleshooting
4
assembly). Remove the entire left part of the detector. Follow the order of
operations in Figure 32. Cover the open end of the PMT assembly to protect
the tube from light.
3. Remove PMT
assembly and
attached parts.
2. Remove two screws
(second screw is on
rear side of chimney).
1. Remove two screws.
Figure 32
Removing the left PMT assembly
To reinstall the vent tube and cover
1 Single-wavelength detector
a Start the two screws on the right side of the cover.
b Start and tighten the screws at the base on the left side.
c Tighten the screws on the right side.
2 Dual-wavelength detector
a Place and support the PMT assembly so that the screw holes line up.
b Install and tighten the four screws.
c Install the cover (two screws).
3 Replace the vent tube assembly.
4 Turn on the GC. Confirm that the flame is off.
5 Restore the operating conditions.
6 Wait 20 minutes for the detector to heat up, then ignite the flame.
FPD Installation and Operation
61
4
Maintenance and Troubleshooting
Replacing the Heater/Sensor Assemblies
Replacing the heater/sensor assemblies takes about 30 minutes. It requires
you to turn off the GC, remove the vent, the detector cover, and, on the
dual-wavelength detector, the left PMT assembly.
CAUTION
When turning the GC off, turn off the flame first to prevent condensation from dripping
into the jet and column.
You may wish to replace or check the FPD heater/sensor assemblies for the
following reasons:
• One or both of the heaters or sensors are defective.
• The actual temperature reading on the display of the heaters is cycling more
than 1 °C.
Materials needed
• G1535-60610 Heater/Sensor assembly with short lead for the emissions
block assembly.
• G1535-60620 Heater/Sensor assembly with long lead for the transfer line.
• ESD protection: For example, a wrist strap
• Wrenches: 8710-0803 (9/16-inch), 8720-0010 (5/8-inch), 1/4-inch × 3/8-inch
• Torx drivers: 8710-2140 T-10 and 8710-1807 T-20.
Procedure
1 Turn off the flame.
2 Turn off the GC.
3 Remove the vent assembly and cover. Refer to “Accessing Heaters and
Ignitor” on page 58.
4 Put on an ESD wrist strap. Remove the right-side cover to access the GC
electronics. Disconnect the heater/sensor leads from the auxiliary heater
board and the connectors above the main board.
5 Carefully pull the cables up onto the top of the GC.
62
FPD Installation and Operation
Maintenance and Troubleshooting
4
Transfer line
1 Use a Torx T-10 driver to remove the screw and retainer clip holding the
lower heater/sensor assembly (Figure 33). Remove the heater and sensor
from the transfer line.
Retainer clip
Figure 33
Transfer line heater/sensor
2 Remove the protective cap from the temperature sensor of the
heater/sensor assembly with the short cable.
FPD Installation and Operation
63
4
Maintenance and Troubleshooting
3 Insert the heater and sensor into the transfer line. Make sure the sensor is
seated at the bottom of the hole. If not, the AUX temperature will wander
above and below the detector setpoint.
Figure 34
64
Install the transfer line heater/sensor
FPD Installation and Operation
Maintenance and Troubleshooting
4
4 Position the retainer clip over the heater/sensor assembly and install the
screw.
Figure 35
Install the retainer clip
Emissions block assembly
1 Remove the upper heater and temperature sensor from the emissions block
assembly.
2 Remove the protective cap from the sensor of the heater/sensor assembly
with the long cable.
FPD Installation and Operation
65
4
Maintenance and Troubleshooting
3 Install the upper heater and sensor in the emissions block assembly.
Figure 36
66
Install the upper heater and sensor
FPD Installation and Operation
Maintenance and Troubleshooting
4
Closing up
1 Route the heater/sensor cables out of the bracket (Figure 37).
Figure 37
Route the heater/sensor cables
2 Replace the cover, vent assembly, and, on the dual-wavelength detector, the
left PMT assembly. Refer to “Accessing Heaters and Ignitor” on page 58.
3 Carefully thread the heater/sensor cables into the electronics compartment.
4 Put on an ESD wrist strap. Connect the short cable as shown in Figure 6 on
page 23. Connect the long cable to the auxiliary heater board (Table 11).
Table 11
Connectors and leads
Detector type
Location
Connector
Single-wavelength
Front
A1
Single-wavelength
Back
A2
Dual-wavelength
Back
A2
FPD Installation and Operation
67
4
Maintenance and Troubleshooting
5 Replace the right-side cover to the GC electronics compartment.
6 Turn on the GC. Confirm that the flame is off.
7 Restore the operating conditions.
8 Wait 20 minutes for the detector to heat up, then ignite the flame.
68
FPD Installation and Operation
4
Maintenance and Troubleshooting
Replacing the Ignitor
Replacing the ignitor takes about 20 minutes. It requires you to turn off the
GC, remove the vent and cover, and, on the dual-wavelength detector, the left
OMT assembly. Agilent recommends that you do not touch these parts with
your bare hands. For optimum performance use lint-free gloves for assembling
and inserting the new parts into the emissions block assembly.
You may wish to replace the FPD ignitor for the following reasons:
• After the detector reaches operating temperatures, the FPD will not light.
• Baseline increase indicates dirt buildup.
Materials needed
• 19256-60800 Ignitor replacement kit
• Wrenches: 1/4-inch × 5/16-inch (8710-0510)
• Torx driver: T-10 (8710-2140)
• 8650-0030 (large) or 8650-0029 (small) Nylon lint-free gloves
The FPD Ignitor replacement kit includes a glow plug, a spacer, and an O-ring.
Do not use the copper ring that ships with the glow plug.
Procedure
1 Turn off the flame.
2 Turn off the GC.
3 Remove the vent assembly, cover, and, on the dual-wavelength detector, the
left PMT assembly. Refer to “Accessing Heaters and Ignitor” on page 58.
FPD Installation and Operation
69
4
Maintenance and Troubleshooting
4 Use a Torx T-10 driver to loosen the collar screw holding the cable assembly
to the ignitor (Figure 38). Remove the collar and cable assembly. Some
FPDs have a version of the collar with two screws.
Figure 38
Removing the ignitor cable
5 Use a wrench to loosen and remove the glow plug. Use tweezers to remove
the O-ring.
70
FPD Installation and Operation
Maintenance and Troubleshooting
4
6 Assemble the parts for the new ignitor (Figure 39).
Glow plug
Spacer
O-ring
Figure 39
Ignitor parts assembled
7 Insert and tighten the parts.
8 Replace the ignitor collar and cable assembly (Figure 40). Some collars have
two screws.
Figure 40
FPD Installation and Operation
Connecting the ignitor cable
71
4
Maintenance and Troubleshooting
9 Replace the cover, the vent tube assembly, and, on the dual-wavelength
detector, the left PMT assembly.
10 Turn on the GC. Confirm that the flame is off.
11 Restore the operating conditions.
12 Wait 20 minutes for the detector to heat up, then ignite the flame.
72
FPD Installation and Operation
Maintenance and Troubleshooting
4
Replacing the Inert Transfer Line
Occasionally, the inert transfer line between the column and the emissions
block must be inspected, cleaned, and/or replaced. Figure 41 shows an
installed inert transfer line.
Cover and cables
removed for clarity
Transfer line assembly
Mounting nuts
Figure 41
Left side of the detector
Removing the transfer line
1 Turn off the flame.
2 Turn off the GC and unplug the power cord. Let the GC cool.
CAUTION
To avoid damaging the photomultiplier tube, always turn the GC or electrometer off
before removing the PMT assembly.
3 Inside the oven, remove the column and adapter (if installed) to the FPD.
4 Locate the gray ignitor cable attached to the side of the detector. Trace the
cable to the signal board and disconnect it there.
FPD Installation and Operation
73
4
Maintenance and Troubleshooting
5 Remove the vent tubing and the sheet metal cover.
Single-wavelength: two screws at the right-side top and two at the left-side
bottom.
Dual-wavelength: two screws at the right-side top.
6 Remove the PMT assemblies (release the spring, then twist and pull). It is
not necessary to disconnect any cables; just place the assemblies on top of
the GC and cover them to protect them from light.
7 Remove the two mounting nuts that hold the transfer line assembly
(Figure 41).
8 Four screws connect the lens holder to the right face of the emissions block
assembly (Figure 42). Loosen, but do not remove, the screws on the bottom
and the two sides.
Similarly, loosen the screws on the left side the lens holder, if present.
Loosen these screws
Figure 42
Lens holder and screws.
9 Grasp the emissions block assembly and carefully lift it straight up. The
transfer line will come with it. Twist and pull to separate the two parts.
If the emissions block assembly/transfer line will not lift free of the detector
bracket, check for tubing or cables catching on the sheet metal.
10 If you will be installing a new transfer line assembly, trace the gas tubing to
the manifold block on the flow module. Remove the single screw that holds
the fitting. Install new O-rings.
74
FPD Installation and Operation
Maintenance and Troubleshooting
4
Reassembly
1 Insert the transfer line into the bottom of the emissions block assembly.
2 Slide the combined parts into the detector body. The semicircular plates
that the three screws connect to go into the gap between the two parts of
the bracket.
3 Install the two mounting nuts that hold the transfer line.
4 Check that the emissions block assembly is fully seated on the transfer line
and that all of the cables and tubing are properly placed.
5 Tighten the screws that secure the lens holders.
6 Install the PMT assemblies).
7 Reconnect the ignitor cable.
8 Install the cover and the vent tube.
9 If necessary, connect the gas lines to the flow module.
10 Restore operating conditions.
11 Wait 20 minutes for the vent tube to heat up, then ignite the flame.
FPD Installation and Operation
75
4
Maintenance and Troubleshooting
Troubleshooting
Offset or detector output too high or too low
Using a filter with flows optimized for the other filter type can cause
unexpected output levels.
Monitor the FPD output. Table 12 provides examples of detector output when
the filter installed in the detector and the gas flows in use do not match.
Table 12
Filter/Flow mismatch
Outputs
Gas flows optimized for
With sulfur filter
With phosphorus filter
Sulfur
30 to 50
10 to 12 (low)
Phosphorus
240 to 250 (high)
30 to 50
Besides having the wrong filter for a particular set of gas flows, also consider:
• If the Lit Offset is 0.5 to 3.0, check that the flame is ON.
• If the Lit Offset is 0, check if the electrometer is turned OFF or the signal
cable is disconnected.
• If the Lit Offset <30, the flame may be in the wrong position. Check detector
flows, column flow, and column position.
MDL too high
Table 13 lists typical MDL values for a checkout.
Table 13
76
Typical MDL values for a checkout
Typical range after 24 hours
Limits at installation
P filter
0.060 to 0.080
≤0.100
S filter
3.8 to 5
≤6
FPD Installation and Operation
Maintenance and Troubleshooting
4
The MDL is dependent on the peak area and the detector noise. The
relationship is: the smaller the peak area and the larger the noise
measurement, the larger the MDL. If the MDL is high, check under the “High
noise level” on page 77 and “Small peak area” on page 77.
High noise level
Table 14 lists typical noise values for a checkout.
Table 14
Typical range of values for a checkout
Typical range after 24 hours
Limits at installation
P filter
1.6 to 3.0
≤4
S filter
2 to 4
≤5
Higher than expected noise is caused by:
• Low purity or contaminated source gases.
• Unconditioned column or ferrules.
• Dirty or contaminated inlet components, such as the liner.
• Dirty or contaminated detector parts, such as the ignitor.
• Light leak at PMT or Vent tube. Turn the flame off and check the output. If
the output is above 10 or 20 pA you probably have a light leak.
Small peak area
Table 15 lists typical peak area values for a checkout.
Table 15
Typical peak area values for a checkout
Typical range after 24 hours
Limits at installation
P filter
19000 to 32000
≥19000
S filter
8000 to 19000
≥8000
FPD Installation and Operation
77
4
Maintenance and Troubleshooting
Small peak area is caused by:
• End of column extends too far into the detector. Sample not burned in
flame.
• Sample lost in inlet or at column connections. Check your GC method split
or splitless setpoints. Check the inlet septum, liner O-ring, and seal.
• Photo-multiplier tube defective.
• Incorrect filter or detector flows.
Large peak width at half-height
Table 16 lists typical peak width values for a checkout.
Table 16
Typical peak width values for a checkout
Typical range after 24 hours
P filter
0.05 to 0.07
S filter
0.06 to 0.08
Large peak width is caused by:
• Activity in the inlet or column.
• Injection volume too large for inlet, liner, or inlet conditions.
Detector Temperature Not Ready (6890)
The performance of the AUX heater is affected by the placement of the PRT
sensor. If it is not seated completely into the transfer line, the temperature will
wander about the set point and the GC will be Not Ready. See Table 17.
Table 17
78
Detector temperature range and duty cycle
PRT location
Setpoint
Duty cycle
Temperature
range
Detector
200 °C
16–17%
200.02 to 199.98 °C
AUX Seated
200 °C
16–24%
200.20 to 199.8 °C
AUX not seated
200 °C
50–100%
205.00 to 195.00 °C
FPD Installation and Operation
Maintenance and Troubleshooting
4
If the AUX temperature for the FPD is cycling or wandering, view the PID
thermal diagnostic for the AUX heater by:
1 On the keypad, press Options.
2 Scroll to and select Diagnostics.
3 Scroll to and select Thermal PID control.
4 Scroll to and select AUX 1 or 2. This allows you to view the temperature
range and duty cycle. Check the table above for normal ranges.
Clipped peaks
If you have an application at the upper limit of the dynamic range (especially
with sulfur), you may have to desensitize your instrument. Replace the
1000-1437 sulfur filter with filter part number 19256-80000. Than set the
detector gas flows to the values used in the phophorus checkout method. This
raises the baseline but with some loss in the signal-to-noise ratio.
FPD Installation and Operation
79
4
Maintenance and Troubleshooting
There should be no problems with either solution and the use of hydrogen.
However, please note the following warning.
WA R N I N G
Hydrogen gas is flammable and potentially explosive. Be sure to turn off the
hydrogen gas at the source until connections are made. Also, leak test connections,
lines and valves before operating or servicing the instrument.
Data lost because detector tries to reignite during a run
Controlling Flame Auto-Ignition
Certain environmental conditions, such as
• Strong electromagnetic fields
• Large ambient temperature swings
• Large atmospheric pressure swings
can cause an artificially low signal in the GC, incorrectly indicating that the
flame has gone out. As a result, the run aborts and the GC tries to relight an
already-lit flame.
You can verify that the flame is lit by holding a cold, shiny surface (such as a
mirror or a wrench) over the exit tube. Condensation on the surface indicates
that the flame is lit.
Reset the Lit Offset to 2.0.
CAUTION
An attempt to relight an already-lit flame corrupts any chromatograms created and
shuts down the GC.
Flame extinguishes after ignition
Condensation in the vent tube because the detector was too cool when the
flame was ignited.
Flame going out is caused by:
• Incorrect detector gas flows for a mix of air and hydrogen.
• Restriction to detector gas flows.
80
FPD Installation and Operation
Maintenance and Troubleshooting
4
• Leak at detector EPC module.
• Condensation dripping onto flame. Prevent this by turning the flame off
until detector is at temperature for 15 minutes.
FPD Installation and Operation
81
4
82
Maintenance and Troubleshooting
FPD Installation and Operation
Agilent G2333B and G2334B Flame Photometric Detectors
Installation and Operation
A
Replacement Parts
Inert Transfer Line 84
FPD Ignitor and Heat Shield Assembly 86
FPD Lens Assembly 88
PMT and Bracket Assemblies 90
Covers, Flow Modules, and Electronics 92
Agilent Technologies
83
A
Replacement Parts
Inert Transfer Line
Table 18
84
Inert transfer line parts (Figure 43)
Item
Description
Part number
1
O-ring, FPD jet seal, white
0905-1608
2
Inert transfer line
19256-60555
3
Heater/Sensor assembly
G1535-60620
4
Capillary adapter seat
19256-21140
5
Capillary adapter nut
19256-21150
6
1/8-inch ferrule
0100-1332
7
1/8-inch nut
5180-4103
8
1/4-inch packed adapter
G1532-20710
9
Screw, M3 × 12 mm
0515-1084
10
Retaining clip
19256-00340
FPD Installation and Operation
Replacement Parts
1
A
3
9
10
2
6
7
4
5
8
Figure 43
Inert transfer line
FPD Installation and Operation
85
A
Replacement Parts
FPD Ignitor and Heat Shield Assembly
Table 19
86
FPD ignitor and heat shield assembly parts (Figure 44)
Item
Description
Part number
1
FPD tube assembly
Aluminum
Stainless Steel
19256-60700
19256-20705
2
Vespel ferrule, 1/4-in ID
0100-1061
3
Emissions block assembly
FPD, single
FPD, dual (not shown)
19256-80560
19256-80600
4
Ignitor replacement kit
A. O-ring
B. Spacer
C. Glow plug
19256-60800
5
Ignitor cable assembly
G1535-60600
6
Heat shield gasket, white
19256-80045
7
First heat shield window
19256-80030
8
Heat shield disk
19256-20580
9
Stainless steel coupling
19256-20550
10
Lock washer (4 required)
2190-0584
11
Screw, M3 × 12 (4 required) - T10
0515-1084
12
Collar
19256-20690
13
Screw, M3 × 66 mm, T-10
0515-0680
FPD Installation and Operation
Replacement Parts
A
1
2
3
4
6
7
8
A
13
12
B
*
9
C
5
* Collar may have one or two screws.
Figure 44
10
11
FPD ignitor and heat shield assembly
FPD Installation and Operation
87
A
Replacement Parts
FPD Lens Assembly
Table 20
88
FPD lens assembly parts (Figure 45)
Item
Description
Part number
1
Clamp
19256-00090
2
Screw, M3 × 25 (4 required)
0515-0683
3
Silicone O-ring, 0.926-in ID (orange)
0905-0955
4
Convex lens
1000-1438
5
Lens housing
19256-20900
6
Flange ring
19256-00200
7
O-ring, Viton, 1.239-in ID (brown), for lens housing
0905-1100
FPD Installation and Operation
Replacement Parts
A
3
4
5
6
1
7
2
Figure 45
FPD lens assembly
FPD Installation and Operation
89
A
Replacement Parts
PMT and Bracket Assemblies
Table 21
90
PMT and Bracket Assemblies Parts (Figure 46)
Item
Description
Part number
1
Chimney back cover
G1535-80520
2
Heater/Sensor assembly
G1535-60610
3
Transfer line support bracket
19256-00320
4
Bracket/Support
G1535-00010
5
5b
Emissions block assembly, single
Emissions block assembly, dual
19256-60650
19256-60690
6
Filters
Sulfur
Phosphorus
1000-1437
19256-80010
7
Filter spacer (used only with sulfur filter)
19256-20910
8
PMT housing assembly
19256-60510
9
Dual FPD chimney front
G1535-00030
10
Dual cover assembly
G1535-80530
11
Dual FPD chimney back
19256-00330
12
Dual main bracket
G1535-00040
FPD Installation and Operation
Replacement Parts
A
1
8
6
7
2
5
3
10
4
5b
11
12
9
Figure 46
PMT and bracket assemblies
FPD Installation and Operation
91
A
Replacement Parts
Covers, Flow Modules, and Electronics
Table 22
Item
Description
Part number
1
FPD assembly
Single wavelength
Dual wavelength (not shown)
G1535-61555
G1535-61565
Top cover
Single wavelength
Dual wavelength
G1535-80555
G1535-80560
3
Flow module kit
G1535-60720
4
Electronics cover pan
G1535-00120
5
Electronics top cover
G1535-80520
6A
6B
6C
Solenoid valve bracket
Aux zone/valve box cable
Screw, M4 × 12 mm (2)
G1580-00070
G1530-60660
1390-1023
7
Signal board
G1535-60010
8
Ground strap
19256-60730
NS
Spring to secure PMT
1460-1160
NS
FPD update kit, single wavelength
FPD update kit, dual wavelength
FPD PM kit, single wavelength
FPD PM kit, dual wavelength
G2647A
G2648A
G2647-60510
G2648-60510
NS
Column measuring tool (see Figure 23 on page 50)
19256-80640
2
92
Covers, manifolds, and electronics parts (Figure 47)
FPD Installation and Operation
Replacement Parts
A
1
3
2
4
5
8
6C
6A
7
6B
Figure 47
Covers, manifolds, and electronics
FPD Installation and Operation
93
A
94
Replacement Parts
FPD Installation and Operation
Agilent Technologies
© Agilent Technologies, Inc.
Printed in USA, May 2005
G1535-90328

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