OI Analytical 5380 User manual

5380
DETECTORCONTROLLER
H
2
AIR 1
AIR 2
FINE
ADJUST
ON
AUX
Model 5380 Pulsed Flame
Photometric Detector (PFPD)
Operator’s Manual
151 Graham Road · P.O. Box 9010 · College Station, Texas 77842-9010 USA
Toll-Free: [phone] • Tel: [phone] • FAX [phone] • www.oico.com

Notice
The information contained in this document may be revised without notice.
OI Analytical shall not be liable for errors contained herein or for incidental, or consequen-
tial, damages in connection with the furnishing, performance, or use of this material.
No part of this document may be reproduced, photocopied, or translated to another lan-
guage without the prior written consent of OI Analytical.
Revision 3.1 — December 2001
OI Analytical Part #283101
Printed in the U.S.A.
Publication 08231201
Copyright 1998–2001 OI Analytical
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Teflon is a registered trademark of E.I. du Pont de Nemous & Co., Inc.

Limited Warranty
OI Analytical warrants each Model 5380 Pulsed Flame Photometric Detector (PFPD)
against defects in materials and workmanship under normal use and service for a period of
ninety (90) days. Equipment installed by OI Analytical is warranted from the installation
date; all other equipment is warranted from the ship date. If purchaser schedules or delays
installation more than 90 days after delivery, then warranty period starts on the 91st day
from date of shipment. This warranty extends only to the original purchaser. OI Analytical
will, at its option, repair or replace equipment that proves to be defective during the
warranty period, provided the equipment is returned to OI Analytical at the expense of the
purchaser. Parts, labor, and return shipment to the customer shall be at the expense of OI
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programming instructions when properly installed on that CPU. OI Analytical does not
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free.
Consumables, columns, lamps, and high temperature furnaces are warranted for 30 days
(parts only) and are not available for coverage under extended warranties or service
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This warranty shall not apply to defects originating from:
Improper maintenance or operation by purchaser.
 Purchaser-supplied accessories or consumable.
Modification or misuse by purchaser.
Operation outside of the envirnonmental and electrical products specifications.
Improper or inadequate site preparation.
Purchaser-induced contamination or leaks.
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TORT, OR OTHERWISE.
Any service requests or questions should be directed to the Customer Service Department
at 1-800-336-1911.

Table of Contents
Chapter 1: Introduction
Detector Design ................................................................................................. 1
Principle of Operation........................................................................................ 1
Features .............................................................................................................. 5
Specifications..................................................................................................... 6
Compliance and Safety Information .................................................................. 8
Chapter 2: Description of Components
Model 5380 Detector Assembly - Assembled View ....................................... 11
Model 5380 Detector Assembly - Exploded View .......................................... 12
Model 5380 Detector Controller - Front View ................................................ 14
Model 5380 Detector Controller - Back View................................................. 15
Chapter 3: Introduction to WinPulse
Overview of Main WinPulse Screen ............................................................... 17
WinPulse Menu System................................................................................... 19
Menu Features.................................................................................................. 20
Secondary WinPulse Screens........................................................................... 22
Chapter 4: Installation
Installing the Model 5380 PFPD Assembly .................................................... 29
Installing the Model 5380 PFPD in the Agilent 6890 Valve Box ................... 32
Installing the Model 5380 Detector Controller................................................ 35
Installing the Pneumatics ................................................................................. 36
Preparing the PFPD for Operation................................................................... 45
Installing the WinPulse Software .................................................................... 52
Chapter 5: Operation
Starting the PFPD System................................................................................ 53
Optimizing the Combustor Flow ..................................................................... 56
Optimizing PFPD Detectivity and Selectivity ................................................. 62
Minimizing Quenching .................................................................................... 68
Detecting Phosphorus and Sulfur Simultaneously .......................................... 68
Testing the PFPD Performance ..................................................................... 69
Recording WinPulse Files to be Viewed with PFPDView.......................... 71
Chapter 6: Maintenance
Changing the Combustor ................................................................................. 73
Testing and Replacing the Ignitor Assembly................................................... 77
Replacing Optical Components ....................................................................... 78
Cleaning the Model 5380 PFPD ...................................................................... 82
Chapter 7: Troubleshooting
Troubleshooting ............................................................................................... 85

Chapter 8: Replacement Parts
Replacement Parts .......................................................................................... 91
Chapter 9: Glossary
Glossary ........................................................................................................... 95
Bibliography
Bibliography .................................................................................................... 99
Appendix A
Photomultiplier Tube and Filter Configurations............................................ 101
Appendix B
Definition of Detectivity ................................................................................ 103
Appendix C
Dual Gate Capability and Calculation of Alpha ............................................ 105
Appendix D
Noise Sources and Output Signal Optimization Guide ................................. 113
Appendix E
Technical Assemblies .................................................................................... 119
Index
Index ............................................................................................................. 121

Chapter 1 1
Introduction
Chapter 1
Introduction
OI Analytical’s Model 5380 Pulsed Flame Photometric Detector (PFPD) is the
latest advance in flame photometric detector design, optimized for the selective
detection of sulfur, phosphorus, and other compounds. The Model 5380 PFPD is
protected under U.S. Patent #5,153,673 and international patents issued to Aviv
Amirav, Tel Aviv University, Israel.
Detector Design
The Model 5380 PFPD consists of four principal components:
• Model 5380 Detector Assembly
• Model 5380 Detector Controller
• Pneumatics (either in the Detector Controller or in the GC)
• WinPulse™Software Program
The Model 5380 Detector Controller houses the signal processing, control, and
power supply electronics. The Detector Assembly consists of the base, combustor,
tower, ignitor cap, ignitor assembly, light pipe, optical filter, photomultiplier tube
(PMT) housing, PMT, heater, and temperature sensor. The pneumatics consist of
three flow controllers, a precision needle valve, and an associated gas manifold.
They are located either in the Detector Controller or within the pneumatics com-
partment of the GC system.
Principle of Operation
Operation of the Pulsed Flame Photometric Detector is based on a propagating
flame that terminates within a fused silica combustor. The gas phase reactions
produced by the propagating flame result in light emissions with specific lumines-
cence spectrum and lifetimes. The differences in specific emission lifetimes
combined with the kinetics of the propagating flame allow both time and wave-
length information to be used to improve the selectivity of the PFPD and to de-
crease the observed noise (which enhances sensitivity). Since a propagating flame
is used, lower combustible gas flow rates are used to increase the relative concen-
tration of the analyte. This is especially important for species, such as sulfur, that
form a dimer. In addition, the use of gated electronics permits the rejection of noise
occurring outside of the specified gate window. This further improves the
detectivity of the PFPD.
In order to retain all the sample compounds in the combustor for increased bright-
ness, a separate secondary flow of air and H2is continuously directed around the
outside of the combustor to separately fill the igniter cap with fresh combustible

2 Model 5380 PFPD Operator’s Manual
Rev. 3.1
gas mixture, which is richer with air for easier ignition. The primary and secondary
gas flows are known as combustor gas (COMB) and wall gas (WALL), respec-
tively. The separate pathways of these two gas mixtures within the detector are
shown schematically in Figure 1.1.
The pulsed flame propagation consists of a four phase cycle: replenishment of
combustible gases, ignition of gases, downward propagation of the flame (combus-
tion), and extinction of the flame (see Figure 1.2). The cycle begins with the
combustor gases (GC effluent, H2, and air) flushing out the combustor. Simulta-
neously, the wall gases (H2and air) sweep spent gases from the ignitor region
through a vent, and fill this space with a combustible gas mixture. The flame is
initiated when this gas mixture reaches the glowing ignitor coil. The flame then
propagates from the ignitor region through a convoluted pathway (to prevent light
from the ignitor reaching the PMT) and down into the combustor. If the gas
composition within the combustor is set correctly, the flame continues to propagate
toward the bottom of the combustor, where it terminates when all the combustor
gas has been consumed.
The pneumatic system of the PFPD has been designed to allow the operator to
regulate both the flow rates and the H2:Air composition of the combustor and wall
gases. Figure 1.3 provides a flow diagram of the pneumatic system. Three manual
or electronic gas flow controllers enable the operator to adjust the flow rates of H2
and air in the combustor gas and wall gas mixtures. The H2and Air 1 control
Figure 1.1. Combustor and Wall Gas Pathways
Ignitor
Vent
Detector Cap
Detector Body
Combustor
Detector Base
Combustor Gas
(H2+ Air 1; H2rich)
Wall Gas
(H2+ Air 1 + Air 2;
Air rich)
GC Effluent
↑
←
←

Chapter 1 3
Introduction
valves determine the composition of the gas mixture supply to the combustor. In
order to achieve rapid and consistent flame initiation at the ignitor, additional air is
added to the wall gas mixture by adjusting the Air 2 control valve. The relative
amounts of the H2:Air 1 gas mixture that flow to the combustor and ignitor regions
are controlled by a fine adjust needle valve.
Figure 1.2. Four Phase Cycle of Propagating Flame
Replenishment Ignition Combustion Extinction
Gas Outlets
Combustor Gas (COMB)
(H2+ Air 1; H2rich)
connects to lower gas line on detector base
Manual or Electronic
Gas Flow Regulators Supply Gas Inlets
H2
Air 1
Air 2
H2IN
Air IN
Wall Gas (WALL)
(H2+ Air 1 + Air 2; Air rich)
connects to upper gas line on detector base
T3 T2
T1
T4
Figure 1.3. Model 5380 PFPD Pneumatics Flow Chart
Spent Gas Wall Gas Combustor Gas

4 Model 5380 PFPD Operator’s Manual
Rev. 3.1
In general, the gas flow controllers are used to optimize the H2:Air ratios in both
the wall and combustor regions while the fine adjust needle valve is used to
regulate the split of the H2:Air 1 mixture between the wall and combustor regions.
The relative rates of the wall and combustor flows can be adjusted so that the time
required to fill the ignitor volume with gas is equal to or slightly greater than the
time required to fill the combustor. If the ignitor fill time is less than the combustor
fill time, flame propagation becomes unstable with the flame alternately terminat-
ing at the top and the bottom of the combustor. This phenomenon is known as
“tick-tock.” Combustion of the GC analyte within the combustor volume is opti-
mized by using the fine adjust needle valve to adjust the detector to the tick-tock
condition and then increasing the combustor flow (or decreasing the ignitor flow)
slightly until the flame terminates only at the bottom of the combustor. This allows
the operator to easily manipulate the kinetics of the propagating flame and the
associated magnitude and lifetime of the chemiluminescence resulting from
combustion. (Refer to Chapter 5, “Operation,” for a discussion of pneumatic
settings that optimize the operating efficiency of the PFPD.)
The emission spectra detected by the PFPD are the product of the transmission of
the emitted photons through the light pipe and filter, and the spectral sensitivity of
the photomultiplier tube. Specific emission bands can be observed for species that
are produced in the PFPD. With a conventional flame photometric detector (FPD),
narrow band pass or interference filters are used to minimize interference from
carbon in the continuous flame. By contrast, the PFPD uses broad band pass filters
and time-based selectivity to minimize interference and increase optical through-
put. The background emission associated with the H2-rich flame in the combustor
consists of CH*, C2*, and OH* species that exist in the flame. While this emission
lasts less than 1 ms, the observed emission time of up to 4 ms (Figure 1.4) is due to
the dynamics of the flame propagating through the combustor. However, the sulfur
emission reaches its maximum 5–6 ms after the background emission is nearly
terminated. Thus sulfur and phosphorus have chemiluminescence lifetimes sub-
Figure 1.4. Carbon, Phosphorus, and ulfur Emission Lifetimes
Sulfur
Phosphorus
Carbon

Chapter 1 5
Introduction
stantially longer than the background analyte-free emission. Improvement in
detectivity (see Appendix B) and selectivity for sulfur and phosphorus is obtained
by using gated integration that rejects the unwanted CH*, C2*, and OH* chemilu-
minescence responses. (Refer to Chapter 5 for further discussion of PFPD opera-
tional parameters settings to optimize chemiluminescence responses.)
Since the PFPD is a pulsed detector (generating pulsed chemiluminescence), the
electronics are significantly different from the traditional FPD electronics. For the
PFPD, the most basic pulsed electronics consist of a fast electrometer, an event
(threshold) detection circuit, and a gated integrator. The output from the photomul-
tiplier tube is initially amplified by a fast electrometer. The subsequent output
signal is then digitized and passed through a gated integrator. The integration
interval is defined by the operator specified gates. The Detector Controller then
converts this electronic signal to an analog signal that is proportional to the inte-
grated signal.
The operator’s ability to optimize the operation of the PFPD is facilitated by the
use of WinPulse, a Windows®-based software package developed by OI Analytical.
WinPulse permits the operator to set up and optimize all of the PFPD’s operating
parameters. After these parameters have been uploaded to the Detector Controller,
the software is no longer required for the continued operation of the PFPD. If the
chromatographic conditions change dramatically, the operator can reactivate
WinPulse to reprogram the operational parameters.
Features
• Ability to “tune” selectivity of the PFPD results in fewer false positive identifi-
cations and decreasing the need for additional sample preparation.
• Improved sensitivity compared to many standard FPDs makes it easier to
detect lower quantities of trace-level contaminants and decreases the need for
sample concentration.
• Saves operational gas costs by using only 10% of the gas flow rate of standard FPDs.
• Equimolar sulfur chemiluminescence response that is independent of a
compound’s molecular structure allows calibration for complex samples.
• Real-time dual analog outputs enable acquisition of information for two
elements simultaneously.
• Optimization possible for up to 28 different elements.
• Automated timed events can be set for most detector parameters, which can
extend the performance range of a detector for a given application and often
minimizes the need for complicated chromatographic solutions to difficult
applications.
• No soot formation as a result of “self-cleaning” design.