Agilent Technologies 8355 Sulfur User manual

Agilent Technologies
Agilent 8355 Sulfur and
8255 Nitrogen
Chemiluminescence
Detectors
User Manual

Notices
© Agilent Technologies, Inc. 2017
No part of this manual may be reproduced
in any form or by any means (including
electronic storage and retrieval or
translation into a foreign language)
without prior agreement and written
consent from Agilent Technologies, Inc. as
governed by United States and
international copyright laws.
Manual Part Number
G3488-90010
Edition
Fifth edition, March 2017
Fourth edition, February 2016
Third edition, December 2015
Second edition, October 2015
First edition, September 2015
Printed in USA or China
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Wilmington, DE 19808-1610 USA
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is provided “as is,” and is subject to
being changed, without notice, in future
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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.
WARNING
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.

8355 SCD and 8255 NCD User Manual 3
Contents
1 Getting Started
Manuals, Information, Tools and Where to Find Them 8
Safety Information 8
Online help 8
Education Opportunities 9
Overview of the 8355 SCD and 8255 NCD 10
Overview of Installation and First Startup 14
2SystemDescription
Specifications 16
8355 SCD 16
8255 NCD 16
MDL calculations 17
Theory of Operation 18
SCD 18
NCD 18
Description of Major Components 20
Burner assembly 20
Ozone generator 22
Reaction cell and photomultiplier tube (PMT) 23
EPC modules 23
Vacuum pump 23
Ozone destruction trap 23
Oil coalescing filter 23
FID adapter (optional) 24
NCD chiller 24
3Operation
Introduction 26
Integrated version 26
Setting Parameters 27
Parameters and ranges 27
Software control 28
GC keyboard control 30
Identifying the detector 30
Detector Stability and Response 31

48355 SCD and 8255 NCD User Manual
Typical Operating Conditions 32
Adjusting the Operating Conditions 33
Start-up 34
Resource Conservation 36
Shutdown 37
Configure Auto Flow Zero on the GC 37
Automatic Configuration of the Detector 39
4 Maintenance
Maintenance Log and Early Maintenance Feedback (EMF) 42
Maintenance Schedule 43
Tracking Detector Sensitivity 44
Consumables and Replacement Parts 45
Exploded Parts View of the SCD 47
Exploded Parts View of the NCD 48
Detector Maintenance Method 49
Attach a Column to the Detector 50
Replace the Inner Ceramic Tube (SCD) 53
Replace the Quartz Tube (NCD) 56
Check the Vacuum Pump Oil 60
Add Vacuum Pump Oil 61
Replace the Vacuum Pump Oil 63
Replace the Ozone Trap 65
Change the Oil Mist Filter 66
Clean the Detector Exterior 67
Calibrate the Flow and Pressure Sensors 68
Updating Firmware 69
5 Troubleshooting
Solving Detector Problems 72
Troubleshooting Table 73
Status Indicator LED 76
Detector Messages 77

8355 SCD and 8255 NCD User Manual 5
Leaks 78
Ozone leaks 78
Hydrogen leaks 78
Oxidizer leaks 78
Checking for hydrogen and oxidizer leaks 79
Power Problems 80
No power 80
Ozone Generation Problems 81
Coking 82
Hydrogen Poisoning 83
Contaminated Gases 84
6 Performance Verification
About Chromatographic Checkout 86
Prepare for Chromatographic Checkout 87
Prepare sample vials 88
Check SCD Performance 89
Check NCD Performance 95

68355 SCD and 8255 NCD User Manual

7
Agilent 8355 SCD and 8255 NCD
User Manual
Agilent Technologies
1
Getting Started
Manuals, Information, Tools and Where to Find Them 8
Overview of the 8355 SCD and 8255 NCD 10
Overview of Installation and First Startup 14
This chapter introduces the Agilent 8355 Sulfur
Chemiluminescence Detector (SCD) and the Agilent 8255
Nitrogen Chemiluminescence Detector (NCD), and provides
details about where to find helpful information and tools, such
as GC manuals, flow calculators, and so forth.

88355 SCD and 8255 NCD User Manual
1Getting Started
Manuals, Information, Tools and Where to Find Them
This manual describes how to operate the 8355 SCD and the
8255 NCD as installed on an Agilent 7890B Gas Chromatograph
(GC). This manual also provides operating recommendations,
maintenance procedures, and troubleshooting. For installation
instructions, see “Overview of Installation and First Startup” on
page 14. To prepare the installation site for a new SCD or NCD,
see the Agilent Site Preparation Guide.
In addition, Agilent provides other manuals, familiarization
information, and help systems for self-paced learning about the
7890B GC. You will need to reference this general GC
information for installation and operation of the detector. The
sections below describe this information and where to find it.
Safety Information
Before proceeding, read the important safety and regulatory
information found in the Agilent Safety and Regulatory
Information manual for the 8355, 8355 S and 8255, 8255 S
Chemiluminescence Detectors.
Online help
In addition to hardware manuals, your GC data system also
includes an extensive online help system with detailed
information, common tasks, and video tutorials on using the
software.

Getting Started 1
8355 SCD and 8255 NCD User Manual 9
Education Opportunities
Agilent has designed customer courses to help you learn how to
use your GC to maximize your productivity while learning about
all of the great features of your new system:
For course details and education opportunities, visit
http://www.agilent.com/chem/education, or call your local Agilent
sales representative.

10 8355 SCD and 8255 NCD User Manual
1Getting Started
Overview of the 8355 SCD and 8255 NCD
Figure 1 through Figure 5 show the controls, parts, and
components of the 8355 SCD and 8255 NCD used or accessed
during installation, operation, and maintenance.
Figure 1 Front view, detectors (SCD and NCD)
Power switch
Status LED
Power switch
Status LED
8355 SCD 8255 NCD

Getting Started 1
8355 SCD and 8255 NCD User Manual 11
Figure 2 Detector back view
Communications
cable
Burner heater
connector
Heater/sensor
connector
Thermocouple
connector
Hydrogen gas input
Oxidizer gas input
Ozone generator
gas input
Vacuum connection
Power connection Vacuum pump
power connection
Through-hole for
sample transfer line

12 8355 SCD and 8255 NCD User Manual
1Getting Started
Figure 3 Detector gas connections
Figure 4 RV5 Vacuum pump
Hydrogen gas input
Oxidizer gas input
Ozone generator
gas input
Upper hydrogen output
(SCD only)
Oxidizer gas output
Lower hydrogen output
Pump oil pan
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DQGÀOWHU
2LOUHWXUQOLQH
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&ODPSKRVH
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plug

Getting Started 1
8355 SCD and 8255 NCD User Manual 13
Figure 5 RV5 Vacuum pump oil sight gage
Oil level
Sight gage
Maximum oil level
mark
Minimum oil level
mark

14 8355 SCD and 8255 NCD User Manual
1Getting Started
Overview of Installation and First Startup
Below is an overview of the installation process. Installation
and service of the detector should only be performed by
Agilent-trained service personnel.
1If not already installed, install the GC and Agilent data
system. (If another detector is present, verify its
performance.)
2Check GC firmware and driver versions and update as
needed.
3Place the detector on the bench. Remove protective caps.
4Prepare the GC. Cool the GC, then turn off and unplug the
power cord. Remove covers.
5Prepare the detector mounting location.
6Unpack the vacuum pump. Remove plugs. Install oil
coalescing filter and ballast.
7Install the vacuum pump.
8Verify the power configuration.
9Install the burner assembly.
10 Connect the supply gases.
11 Connect the detector gases.
12 Connect the detector cables and wires.
13 Connect cables to the GC and detector.
14 Connect to power.
15 Install the column.
16 Install the GC covers.
17 Turn on the GC and the detector.
18 Configure the detector.
19 Create a checkout method and verify performance.

15
Agilent 8355 SCD and 8255 NCD
User Manual
Agilent Technologies
2
System Description
Specifications 16
Theory of Operation 18
Description of Major Components 20
This chapter provides typical performance specifications, and
describes the theory of operation for the 8355 SCD and 8255
NCD.

16 8355 SCD and 8255 NCD User Manual
2System Description
Specifications
This section lists the published specifications for a new
detector, installed on a new Agilent 7890B GC, when used in a
typical laboratory environment. The specifications apply to the
Agilent checkout sample.
8355 SCD
SCD specifications apply only when using air as the oxidizer
gas.
8255 NCD
Specification
Minimum Detection Limit (MDL),
typical
< 0.5 pg (S)/s (2x Agilent data system
ASTM noise)
Linearity > 104
Selectivity > 2 x 107response S/response C2
Precision*and stability
*Typically, based on one run per 30 minutes, collected over 24 hours. For example, a 24
hour time span will contain approximately 48 replicate runs.
< 2 % RSD over 2 hours
< 5 % RSD over 24 hours
Typical time to reach 800 °C from
ambient
10 min
Specification
Minimum Detection Limit, typical < 3 pg (N)/s (2x Agilent data system
ASTM noise)
Linearity > 104
Selectivity > 2 x 107response N/response C
Area repeatability < 1.5 % RSD over 8 hours
< 2 % RSD over 18 hours
Typical time to reach 900 °C from
ambient
10 min

System Description 2
8355 SCD and 8255 NCD User Manual 17
MDL calculations
The MDL specifications are defined using the Agilent checkout
standard for SCD or NCD.
Sensitivity is typically reported as:
Calculate a minimum detection limit (MDL) from the following
formula:
where the noise is the ASTM noise reported by the Agilent data
system.
Sensitivity = peak area
amount
MDL = 2 x noise
sensitivity

18 8355 SCD and 8255 NCD User Manual
2System Description
Theory of Operation
The SCD and NCD chemiluminescence detectors detect target
molecules by chemically transforming them in several steps to
an excited species that emits light. The light from this emission
is converted to an electrical signal by a photomultiplier tube
(PMT). For each detector, samples undergo preliminary
reaction(s) with an oxidizer (air or oxygen for SCD, oxygen for
NCD) and hydrogen in a very hot reaction zone (the burner) at
reduced pressure to form either SO or NO in addition to other
products such as H2O and CO2. The reaction products then flow
to a reaction cell in a separate detector module. In this cell, they
mix with ozone (O3) produced from oxygen using an ozone
generator. The O3reacts with SO or NO to generate SO2* and
NO2* respectively. This reaction cell operates at a pressure of
about 4-7 Torr. These high energy species return to ground state
by chemiluminescence. The emitted light is filtered and then is
detected by a PMT. The electrical signal produced is
proportional to the amount of SO2* or NO2* formed in the
reaction cell. The sample exits the reaction cell, passes through
an ozone destruction trap, and then passes through a vacuum
pump and out to vent.
SCD
The SCD uses the chemiluminescence (light-producing reaction)
from the reaction of ozone with sulfur monoxide (SO) produced
from combustion of the analyte:
The pressure differential produced by a vacuum pump transfers
the combustion products into a reaction cell, where excess
ozone is added. Light (h) produced from the subsequent
reaction is optically filtered and detected with a blue-sensitive
photomultiplier tube, and the signal is amplified for display or
output to a data system.
NCD
The NCD uses the chemiluminescence of ozone with nitric oxide
formed from combustion. Reacting nitric oxide with ozone
results in the formation of electronically excited nitrogen
dioxide. The excited nitrogen dioxide emits light, a
chemiluminescence reaction, in the red and infrared region of
SO + H2O + other products
Sulfur compound (analyte)
SO + O3SO2+ O2+ hQ(< 300-400 nm)

System Description 2
8355 SCD and 8255 NCD User Manual 19
the spectrum. The light emitted is directly proportionally to the
amount of nitrogen in the sample:
The light (h) emitted by the chemical reaction is optically
filtered and detected by a PMT. A chiller cools the PMT to
reduce thermal noise and help measure infrared light. The
signal from the PMT is amplified for display or output to a data
system.
NO + O
3
NO
2
+ O
2
NO + O
3
NO
2
+ O
2
+ hQ(~600 to 3,000 nm)

20 8355 SCD and 8255 NCD User Manual
2System Description
Description of Major Components
Burner assembly
The burner assembly mounts on top of the GC in a detector
location, and contains the column connection.
For the SCD, the burner provides two heated zones, one at the
base and one farther up the assembly. In the burner base region,
the column effluent mixes with the lower hydrogen flow and air
or oxygen at high temperature. The resulting hydrogen flame
combusts the effluent. Low concentration components burn to
form the usual combustion products, including SO2for
compounds containing sulfur. The products are drawn upward
through a ceramic tube, where at even higher temperature the
upper hydrogen flow mixes with the combustion products,
causing the SO2to reduce into SO.