Agilent 8355 S Sulfur

and 8255 S Nitrogen

Chemiluminescence
Detectors

User Manual

Agilent Technologies
Notices
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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 S SCD and 8255 S NCD 10
Overview of Installation and First Startup 14

2 System Description
Specifications 16
8355 S SCD 16
8255 S 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

3 Keypad Operation
The Detector Key 26
The Status Key 27
The Info Key 28
The General Data Entry Keys 29
Method Storage Keys 30
To load a method 30
To store a method 30

8355 S SCD and 8255 S NCD User Manual 3

 The Service Mode Key 32
The Supporting Keys 33
Configuration 33
Maintenance and System Event Logs 34

4 Operation
Introduction 36
Standalone version 36
Setting Parameters 37
Parameters and ranges 37
Detector Stability and Response 38
Typical Operating Conditions 39
Adjusting the Operating Conditions 40
Start-up 41
Shutdown 42
Flow and Pressure Sensors 43
Flow sensors 43
Pressure sensors 43
Configure auto flow zero 43
Conditions for zeroing a sensor 43
Zero a specific flow or pressure sensor 44
Signal Output 45
Signal Types 45
Value 46
Analog Signals 46
Methods 48
To load a method 48
To store a method 48
Resource Conservation 49
Schedule 49
Sleep Methods 49
To Set the Detector to Conserve Resources 50

5 Maintenance
Maintenance Schedule 54
Tracking Detector Sensitivity 55

4 8355 S SCD and 8255 S NCD User Manual

 Consumables and Replacement Parts 56
Exploded Parts View of the SCD 58
Exploded Parts View of the NCD 59
Detector Maintenance Method 60
Attach a Column to the Detector 61
Replace the Inner Ceramic Tube (SCD) 64
Replace the Quartz Tube (NCD) 67
Check the Vacuum Pump Oil 71
Add Vacuum Pump Oil 72
Replace the Vacuum Pump Oil 74
Replace the Ozone Trap 76
Change the Oil Mist Filter 77
Clean the Detector Exterior 78
Calibrate the Flow and Pressure Sensors 79

6 Troubleshooting
Solving Detector Problems 82
Troubleshooting Table 83
Status Indicator LED 86
Detector Messages 87
Leaks 88
Ozone leaks 88
Hydrogen leaks 88
Oxidizer leaks 88
Checking for hydrogen and oxidizer leaks 89
Power Problems 90
No power 90
Ozone Generation Problems 91
Coking 92
Hydrogen Poisoning 93
Contaminated Gases 94

7 Performance Verification
About Chromatographic Checkout 96

8355 S SCD and 8255 S NCD User Manual 5

 Prepare for Chromatographic Checkout 97
Prepare sample vials 98
Check SCD Performance 99
Check NCD Performance 105

6 8355 S SCD and 8255 S NCD User Manual

Agilent 8355 S SCD and 8255 S NCD
User Manual

1
Getting Started
Manuals, Information, Tools and Where to Find Them 8
Overview of the 8355 S SCD and 8255 S NCD 10
Overview of Installation and First Startup 14

This chapter introduces the Agilent 8355 S Sulfur

Chemiluminescence Detector (SCD) and the Agilent 8255 S
Nitrogen Chemiluminescence Detector (NCD), and provides
details about where to find helpful information and tools, such
as GC manuals, flow calculators, and so forth.

Agilent Technologies 7
1 Getting Started

Manuals, Information, Tools and Where to Find Them

This manual describes how to operate the Agilent 8355 S Sulfur
Chemiluminescence Detector (SCD) and the Agilent 8255 S
Nitrogen Chemiluminescence Detector (NCD). 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 it’s
current line of GCs. 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.

8 8355 S SCD and 8255 S NCD User Manual

 Getting Started 1

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.

8355 S SCD and 8255 S NCD User Manual 9

1 Getting Started

Overview of the 8355 S SCD and 8255 S NCD

Figure 1 through Figure 5 show the controls, parts, and
components of the 8355 S SCD and 8255 S NCD used or
accessed during installation, operation, and maintenance.

Status LED Status LED

Display Display

Keypad
Keypad

Power switch Power switch

8355 S SCD 8255 S NCD

Figure 1 Front view, Standalone detectors (SCD and NCD)

10 8355 S SCD and 8255 S NCD User Manual

 Getting Started 1

Burner heater Hydrogen gas input

connector
Oxidizer gas input

Heater/sensor
connector Ozone generator
gas input
Through-hole for
Analog signal out
sample transfer line
APG Remote
(Readiness only)

Thermocouple
connector

LAN

Vacuum connection

Vacuum pump
Power connection power connection

Figure 2 Standalone detector back view

8355 S SCD and 8255 S NCD User Manual 11

1 Getting Started

Upper hydrogen output

Hydrogen gas input (SCD only)
Oxidizer gas input Oxidizer gas output
Ozone generator Lower hydrogen output
gas input

Figure 3 Standalone detector gas connections

7UDSR]RQH
9DFXXPKRVH

&ODPSKRVH &ODPSKRVH
&ODPSYDFXXP
2LOPLVWÀOWHUDVVHPEO\
DQGÀOWHU
6XSSRUWEUDFNHW
2LOUHWXUQOLQH
9DFXXPKRVH

2LOÀOOFDS

9ROWDJHFRQÀJXUDWLRQ 3RZHUFRQQHFWLRQ
plug Pump oil pan

Figure 4 RV5 Vacuum pump

12 8355 S SCD and 8255 S NCD User Manual

 Getting Started 1

Maximum oil level

mark

Sight gage

Oil level

Minimum oil level

mark

Figure 5 RV5 Vacuum pump oil sight gage

8355 S SCD and 8255 S NCD User Manual 13

1 Getting 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.
1 Place the detector on the bench. Remove protective caps.
2 Prepare the detector mounting location.
3 Unpack the vacuum pump. Remove plugs. Install oil
coalescing filter and ballast.
4 Install the vacuum pump.
5 Prepare the detector.
6 Cool the GC oven, inlet, and other heated zones to a safe
handling temperature (< 40 °C). Turn off the GC.
7 Verify the power configuration.
8 Install the burner assembly.
9 Connect the supply gases.
10 Connect the detector gases.
11 Connect the detector cables and wires.
12 Connect cables to the GC and detector.
13 Connect to power.
14 Install the column.
15 Turn the power on to the detector.
16 Configure the detector.
17 Create a checkout method and verify performance.

14 8355 S SCD and 8255 S NCD User Manual

Agilent 8355 S SCD and 8255 S NCD
User Manual

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 S SCD and
8255 S NCD Detectors.

Agilent Technologies 15
2 System Description

Specifications
This section lists the published specifications for a new
detector, installed on a new Agilent GC, when used in a typical
laboratory environment. The specifications apply to the Agilent
checkout sample.

8355 S SCD

Specification
Minimum Detection Limit (MDL), < 0.5 pg (S)/s (2x Agilent data system
typical ASTM noise)
Linearity > 104
Selectivity > 2 x 107 response S/response C2
Precision* and stability < 2 % RSD over 2 hours
< 5 % RSD over 24 hours
Typical time to reach 800 °C from 10 min
ambient
*
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.

SCD specifications apply only when using air as the oxidizer

gas.

8255 S NCD

Specification
Minimum Detection Limit, typical < 3 pg (N)/s (2x Agilent data system
ASTM noise)
Linearity > 104
Selectivity > 2 x 107 response N/response C
Area repeatability < 1.5 % RSD over 8 hours
< 2 % RSD over 18 hours
Typical time to reach 900 °C from 10 min
ambient

16 8355 S SCD and 8255 S NCD User Manual

 System Description 2

MDL calculations
The MDL specifications are defined using the Agilent checkout
standard for SCD or NCD.
Sensitivity is typically reported as:

peak area
Sensitivity =
amount

Calculate a minimum detection limit (MDL) from the following

formula:

2 x noise
MDL =
sensitivity

where the noise is the ASTM noise reported by the Agilent data
system.

8355 S SCD and 8255 S NCD User Manual 17

2 System 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 O3 reacts 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:

Sulfur compound (analyte) SO + H2O + other products

SO + O3 SO2 + O2 + hQ (< 300-400 nm)

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

18 8355 S SCD and 8255 S NCD User Manual

 System Description 2

the spectrum. The light emitted is directly proportionally to the

amount of nitrogen in the sample:

NO + O3 NO2 + O2

NO + O3 NO2 + O2 + hQ(~600 to 3,000 nm)

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.

8355 S SCD and 8255 S NCD User Manual 19

2 System 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 SO2 for
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 SO2 to reduce into SO.

20 8355 S SCD and 8255 S NCD User Manual

 System Description 2

Figure 6 shows the flow paths for the SCD burner assembly.

Upper hydrogen

Ceramic tube,
upper

Burner

Ceramic tube,
lower

Oxidizer
Base heater Lower hydrogen

Column
&ROXPQÁRZ

Figure 6 SCD flows

For the NCD, 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 hydrogen and air at high
temperature. The resulting hydrogen flame combusts the
effluent. Low concentration components will burn to form the
usual combustion products, including NO2 for compounds
containing nitrogen. The products are drawn upward through a
quartz tube and catalyst, where a high temperature will convert
NO2 into NO.

8355 S SCD and 8255 S NCD User Manual 21

2 System Description

Figure 7 shows the flow paths for the NCD burner assembly.

To detector

Quartz tube

Burner

Oxidizer
Base heater Hydrogen

Column

&ROXPQÁRZ
Figure 7 NCD Flows

Ozone generator
The ozone generator provides ozone that reacts with any SO or
NO in the reaction cell to generate SO2* and NO2* respectively.
These high energy species return to ground state by
chemiluminescence.

22 8355 S SCD and 8255 S NCD User Manual

 System Description 2

The detector regulates the ozone gas supply pressure to

maintain a fixed flow from the ozone generator.

Reaction cell and photomultiplier tube (PMT)

The ozone generator discharges ozone into the reaction cell.
This ozone reacts with any SO or NO to generate SO2* and NO2*
respectively. As the species return to ground state though
chemiluminescence, the photomultiplier tube produces a
current proportional to the intensity of emitted light. A
bandpass filter is used to optimize the detector for either sulfur
or nitrogen detection.

EPC modules
The detector controls hydrogen, oxidizer (air or oxygen), and
ozone supply (oxygen) gas flows using two electronic pressure
control modules.

Vacuum pump
A two-stage, oil-sealed rotary vacuum pump provides an
operating pressure between 3 and 10 Torr in the reaction cell.
This vacuum helps transfer combustion gases from the burner
to the reaction cell, as well as transferring the ozone from the
ozone generator into the reaction cell. The vacuum pump also
reduces non-radiative collisional quenching of the emitting
species in the reaction cell.

Ozone destruction trap

A chemical trap between the detector exhaust and the vacuum
pump destroys ozone, converting it to diatomic oxygen.
Unconverted ozone reduces pump life.

Oil coalescing filter

The oil-sealed rotary vacuum pump uses a partially-open gas
ballast to aid in the elimination of water produced in the burner
and transferred to the pump. As a result of the open gas ballast
and the relatively high flow rates of gases, oil vaporized in the
pump can escape through the pump exhaust. To minimize oil
loss, the pump includes an oil coalescing filter on the pump
exhaust to trap vaporized oil and to return this oil to the
vacuum pump oil reservoir.

8355 S SCD and 8255 S NCD User Manual 23

2 System Description

FID adapter (optional)

The SCD burner normally mounts onto the GC oven directly as a
stand-alone detector. However, some applications also require
simultaneous detection of hydrocarbon components using a
single column without splitting. For this reason, Agilent offers
an optional FID adapter to mount the burner assembly onto an
FID for the simultaneous collection of FID and SCD
chromatograms. During dedicated SCD operation, 100 % of the
column effluent passes through the burner to the detector.
During simultaneous detection, approximately 10 % of the FID
exhaust gases are drawn into the burner through a restrictor,
which reduces SCD sensitivity to approximately 1/10 of the
signal observed in a dedicated SCD burner.

NCD chiller
For NCD, the detector uses a Peltier cooler to lower the PMT
temperature, which in turn reduces noise. This chiller cools the
PMT relative to the current ambient temperature. Higher
laboratory ambient temperatures may result in higher PMT
temperatures. Fluctuations in ambient temperature may result
in fluctuations in PMT temperature.
Since noise and response determine the MDL, the efficiency of
the chiller can influence the MDL. Depending on the ambient
temperature, the chiller may not be able to maintain a
sufficiently cool temperature in the PMT, and XCD noise will
increase, therefore increasing the MDL.
Because chiller efficiency depends on the ambient temperature
inside the detector and in the laboratory, the chiller setpoint
does not impact detector readiness. A GC run can start
regardless of whether or not the chiller has cooled to its
setpoint.

24 8355 S SCD and 8255 S NCD User Manual

8355 S SCD and 8255 S NCD
User Manual

3
Keypad Operation
The Detector Key 26
The Status Key 27
The Info Key 28
The General Data Entry Keys 29
Method Storage Keys 30
The Service Mode Key 32
The Supporting Keys 33

This section describes the basic operation of the Agilent

8355 S SCD and 8255 S NCD Detectors keypad.

Agilent Technologies 25
3 Keypad Operation

The Detector Key

These keys are used to set the temperatures, pressures, flows,
and other method operating parameters for the detector.
To display the current settings, press [Det] or [Analog Out]. More
than three lines of information may be available. Use the scroll
keys to view additional lines, if necessary.
To change settings, scroll to the line of interest, enter the
change, and press [Enter].
For context-sensitive help, press [Info]. For example, if you
press [Info] on a setpoint entry, the help provided would be
similar to: Enter a value between 0 and 350.

[Det] Controls detector operating conditions.

[Analog Out] Controls range attenuation and zero offset.

26 8355 S SCD and 8255 S NCD User Manual

 Keypad Operation 3

The Status Key

Displays Ready, Not ready, and Fault information.
The order in which items appear in the scrolling display
window for [Status] can be modified. You may, for example,
want to display the things you most frequently check in the top
three lines so that you do not need to scroll to see them. To
change the order of the Status display:
Press [Config]. Scroll to Status and press [Enter].
Scroll to the setpoint you want to appear first and press
[Enter]. This setpoint will now appear at the top of the list.
Scroll to the setpoint you want to appear second and press
[Enter]. This setpoint will now be the second item on the list.
Continue as above until the list is in the order you require.

8355 S SCD and 8255 S NCD User Manual 27

3 Keypad Operation

The Info Key

Provides help for the currently shown parameter. In other cases,
[Info] will display definitions or actions that need to be
performed.

28 8355 S SCD and 8255 S NCD User Manual

 Keypad Operation 3

The General Data Entry Keys

[Mode/Type] Accesses a list of possible parameters associated with a

component’s nonnumerical settings.

[Clear] Removes a misentered setpoint before pressing [Enter]. It

can also be used to return to the top line of a multiline
display, return to a previous display, cancel a function during
a method, or cancel loading or storing methods.

[Enter] Accepts changes you enter or selects an alternate mode.

Scrolls up and down through the display one line at a time.

The < in the display indicates the active line.

Numeric keys Are used to enter settings for the method parameters. (Press
[Enter] when you are finished to accept the changes.)

[On/Yes] These keys are used to set parameters, such as turning the
[Off/No] pump on, high voltage on.

8355 S SCD and 8255 S NCD User Manual 29

3 Keypad Operation

Method Storage Keys

These keys are for loading and storing methods locally on your
detector. They cannot be used to access methods stored by your
Agilent data system.

[Load] Used together to load and store methods on your detector.

[Method] For example, to load a method, press [Load] [Method] and
[Store] select one from the list of methods stored in the GC.

[Delete] Deletes methods. 

[Sleep/Wake] The detector stores a schedule, based on the on-board clock,

along with two special methods called SLEEP and WAKE. See
“Resource Conservation” on page 49 for additional
information.

To load a method
1 Press [Load].
2 Press [Method].
3 Enter the number of the method to be loaded.
4 Press [On/Yes] to load the method and replace the active
method. Alternatively, press [Off/No] to return to the stored
methods list without loading the method.

To store a method
1 Ensure that the proper parameters are set.
2 Press [Method].
3 Scroll to the method to store, then press [Enter].

30 8355 S SCD and 8255 S NCD User Manual

 Keypad Operation 3

4 Press [On/Yes] to store the method and replace the active

method. Alternatively, press [Off/No] to return to the stored
methods list without storing the method.

8355 S SCD and 8255 S NCD User Manual 31

3 Keypad Operation

The Service Mode Key

Is used to set up Early Maintenance Feedback and to access
inlet leak checks for selected inlet types. This key accesses
settings intended for service personnel. Because these advanced
settings can cause problems if misused, avoid the service
settings unless specifically directed to use them.Is used to
access maintenance functions and settings, service counters,
and diagnostics for the GC.

To view the ozone flow rate, press [Service Mode]. Scroll to

Diagnostics, press [Enter], then select Diag 03 Generator.

32 8355 S SCD and 8255 S NCD User Manual

 Keypad Operation 3

The Supporting Keys

Three logs are accessible from the keypad: the run log, the maintenance
log, and the system event log.
[Logs] Access the Maintenance Log, and the System Event Log. The
information in these logs can be used to support Good
Laboratory Practices (GLP) standards.

[Options] Accesses the instrument parameters setup options for

calibration, communications, and the display. Scroll to the
desired line and press [Enter] to access the associated entries.

[Config] Accesses the detector for configuration and time settings.

[Prog] Use to program a series of keystrokes commonly for specific

[User Key1] operations. Press [Prog] [User Key 1] or [Prog] [User Key 2] to
[User Key2] record up to 21 keystrokes as a macro.

Configuration

Ignore Ready=
To ignore an element's readiness, press [Config] and scroll to
Detector and press [Enter]. Scroll to Ignore Ready and press
[On/Yes] to set it to True.

To set time and date

1 Press [Config] and scroll to Time and press [Enter].
2 Select Time zone (hhmm) and enter the local time offset
from GMT using a 24 hour format.
3 Select Time (hhmm) and enter the local time.
4 Select Date (ddmmyy) and enter the date.

8355 S SCD and 8255 S NCD User Manual 33

3 Keypad Operation

Maintenance and System Event Logs

Two logs are accessible from the keypad: the run log and the
system event log. To access the logs, press [Logs] then scroll to
the desired log and press [Enter]. The display will indicate the
number of entries the log contains. Scroll through the list.

Maintenance logs
The maintenance log contains entries made by the system when
any of the user-defined component counters reach a monitored
limit. The log entry contains a description of the counter, its
current value, the monitored limits, and which of its limits has
been reached. In addition, each user task related to the counter
is recorded in the log, including resetting, enabling or disabling
monitoring, and changing limits or units (cycles or duration).

System event log

The system event log records significant events during the
detector’s operation. Some of the events also appear in the run
log if they are in effect during a run.

34 8355 S SCD and 8255 S NCD User Manual

Agilent 8355 S SCD and 8255 S NCD
User Manual

4
Operation
Introduction 36
Setting Parameters 37
Detector Stability and Response 38
Typical Operating Conditions 39
Adjusting the Operating Conditions 40
Start-up 41
Shutdown 42
Flow and Pressure Sensors 43
Signal Output 45
Methods 48
Resource Conservation 49
This chapter describes the how to use the 8355 S SCD and
8255 S NCD detectors. This chapter assumes familiarity with
detector keypad and display.

Agilent Technologies 35
4 Operation

Introduction

Standalone version
Use the front keypad on the 8355 S SCD or the 8255 S NCD
detector to access the operating parameters. The settings and
information provided on the detector keypad include:
• Settings for temperatures, flows, and gas types
• Sequence integration
• Method storage

36 8355 S SCD and 8255 S NCD User Manual

 Operation 4

Setting Parameters
This section lists the parameter ranges for the SCD and NCD.
The available setpoints provide a wide range suitable for a large
variety of applications as well as for method development. See
“Adjusting the Operating Conditions” on page 40 for important
details about the relationships between the setpoints.

Parameters and ranges

The table below lists the available parameters for the detector.

Table 1 8355 S SCD and 8255 S NCD parameters and ranges

Parameter Range, SCD Range, FID-SCD Range, NCD

Method
Base temperature 125 – 400 °C 125 – 400 °C 125 – 400 °C
Burner temperature 100 – 1000 °C 100 – 1000 °C 100 – 1000 °C
*
Chiller temperature (NCD only) On/Off
Lower hydrogen flow 5 – 25 mL/min — 1 – 25 mL/min
Upper hydrogen flow (SCD only) 25 – 100 mL/min 25 – 100 mL/min —
Oxidizer flow 25 – 150 mL/min. (Air) 5 – 100 mL/min, (Air) 4 – 80 mL/min
5 – 30 mL/min. (Oxygen) 5 – 30 mL/min, (Oxygen)
O3 Generator flow On/Off On/Off On/Off
O3 Generator power On/Off On/Off On/Off
Vacuum pump On/Off On/Off On/Off
* Chiller (PMT cooler) operation depends on the current detector ambient temperature. The actual chiller temperature does not impact
detector readiness. See “NCD chiller” on page 24.

Note that PMT voltage is fixed at 800 V.

8355 S SCD and 8255 S NCD User Manual 37

4 Operation

Detector Stability and Response

The time required for system stabilization varies depending on
the application, system cleanliness, the presence of active sites,
and other factors.
• When starting an existing system, typically wait at least
10 minutes before using the system to collect data.
• A new burner or a new set of ceramic tubes may take up to
24 hours to condition. Set the detector to the operating
conditions, and monitor the baseline until the baseline
becomes stable enough for your application.

38 8355 S SCD and 8255 S NCD User Manual

 Operation 4

Typical Operating Conditions

Table 2 lists the recommended starting conditions for SCD and
NCD methods. These conditions should provide acceptable
results for a wide variety of applications. However, optimize
these conditions as needed to improve the performance of the
specific application.

Table 2 Typical operating conditions, SCD and NCD

Parameter SCD NCD

Base temperature, °C 250 250
Burner temperature, °C 800 900
Chiller temperature N/A On
Upper H2 flow, mL/min 40 N/A
Lower H2 flow, mL/min 10 3
Oxidizer flow, mL/min 50 (Air) 8 (Oxygen)
10 (Oxygen)
O3 Generator flow, mL/min On On
O3 Generator power On On
Vacuum pump On On
Burner pressure, Torr, typical reading <450 Torr, Air < 120 Torr
<300 Torr, Oxygen
Reactor pressure, Torr (read only) Should be below Should be below
7 Torr 5 Torr

The checkout methods for the SCD and NCD also provide
example parameters for balancing good detection limit, good
selectivity, and reasonable ceramic tube life. In any XCD
method:
• Always keep oxidizer gas flowing through the burner.
• The firmware will not allow hydrogen to flow into the burner
while there is no oxidizer to protect the system.
During startup and shutdown, always turn on the pump first
and turn off the pump last to prevent contamination or damage.

8355 S SCD and 8255 S NCD User Manual 39

4 Operation

Adjusting the Operating Conditions

Table 1 on page 37 lists the range of values for each parameter,
as limited by the GC firmware.Table 1 on page 37 lists the range
of values for each parameter, as limited by the detector
firmware. To provide flexibility during method development for
particular application, the range is wider than needed for most
applications.
However, hydrogen flows in the SCD need particular attention.
Using very high hydrogen flows (both upper and lower), relative
to the oxidizer flow, can permanently damage the ceramic
tubes. This condition may not be recoverable. See “Hydrogen
Poisoning” on page 93.
SCD lower hydrogen flow: Very high flow can damage the
ceramic tubes.
NCD lower hydrogen flow: The NCD can operate without
hydrogen flow, although this is not recommended. The hydrogen
flame/plasma can help burn off solvent and heavy molecules. If
operating an NCD without hydrogen flow, plumb the 1/16-inch
tubing for the lower hydrogen flow to the oxygen supply.
Otherwise, residual hydrogen in the tubing will continue diffuse
into the burner and affect stability.
1 Disconnect the Lower H2 line from the back of the detector
and cap off the detector fitting.
2 Install a 1/16-inch Swagelok Tee fitting in the Oxidizer output
from the detector body.
3 Connect the Oxidizer and Lower H2 lines to the Tee fitting.

You will typically need to adjust the recommended starting

conditions to create an optimized method for your application.
When optimizing SCD or NCD method parameters, consider the
following:
• A higher hydrogen to oxidant ratio may initially show higher
response, but later yield a reduced response because of the
accumulation of contaminants that reduce detector
response, such as soot or other active species.
• Operating the burner at higher temperatures may shorten
the useful lifetimes of the heater, thermocouple, and seal
materials.
In general, when making any parameter change, allow sufficient
time for the system to reach equilibrium. Monitor the baseline
until it stabilizes at its new value.

40 8355 S SCD and 8255 S NCD User Manual

 Operation 4

Start-up
How to start the detector depends on whether or not you have
created a method for the detector.
If a valid method exists: After you have used the SCD/NCD (at
least one valid method exists), start the detector by loading the
method. As soon as the method loads, the GC will turn on the
vacuum pump and oxidizer flows, and also turn on all other
parameters except hydrogen flow. The GC will monitor the
temperatures and prevent hydrogen flow until the base
temperature reaches 150 °C and the burner temperature
reaches 200 °C. Once the detector temperatures reach these
minimum limits, the GC turns on the hydrogen flow.As soon as
the method loads, the detector will turn on the vacuum pump
and oxidizer flows, and also turn on all other parameters except
hydrogen flow. The detector will monitor the temperatures and
prevent hydrogen flow until the base temperature reaches
150 °C and the burner temperature reaches 200 °C. Once the
detector temperatures reach these minimum limits, the detector
turns on the hydrogen flow.
During initial startup, or whenever there are no method
parameters set for the SCD or NCD, start the detector as
follows:
1 Access the method parameters.
• At the detector front panel, press [Det].
2 Turn on the vacuum pump.
3 Set the oxidizer flow rate and turn on the oxidizer flow.
4 Wait 1–2 minutes for the vacuum pump to purge the system
using the oxidizer flow.
5 Set the base temperature and turn it on.
6 Set the burner temperature and turn it on.
7 For NCD only: Set the chiller temperature and turn it on.
8 Set the hydrogen flow and turn it on.
9 Set the ozone generator supply gas flow and turn it on.
10 Turn on the ozone generator power.

The detector will monitor the temperatures and prevent

hydrogen flow until the base temperature reaches 150 °C and
the burner temperature reaches 200 °C. Once the detector
temperatures reach these minimum limits, the detector turns on
the hydrogen flow.

8355 S SCD and 8255 S NCD User Manual 41

4 Operation

Shutdown
When turning off the detector for a long period of time, or to
perform maintenance on the GC or detector, shut down the
detector as follows:
1 Access the method parameters.
• At the detector keypad, press [Det].
2 Turn off the ozone generator power.
3 Turn off the ozone generator supply gas flow.
4 Turn off all hydrogen flows.
5 For NCD only: Turn off the chiller.
6 Turn off the burner heater.
7 Turn off the base heater.

When shutting down, the detector will keep the vacuum pump and
NOTE
oxidizer flow running until approximately 100 mL of oxidizer gas has
purged the system after the hydrogen flow is turned off. This action
prevents moisture residual contamination.

8 Turn off the oxidizer flow.

9 Turn off the vacuum pump.
10 Turn off the detector power.
11 If shutting down the GC, turn off the GC.

WA RNING Burn hazard. Many parts of the detector can be dangerously hot.
If performing detector maintenance, turn off all heated zones and
monitor them until they reach a safe handling temperature before
turning off the GC and detector.

Alternately, create a method that turns off all detector

components, and load that method to shut down the detector.

42 8355 S SCD and 8255 S NCD User Manual

 Operation 4

Flow and Pressure Sensors

The EPC gas control modules contain flow and/or pressure
sensors that are calibrated at the factory. Sensitivity (slope of
the curve) is quite stable, but zero offset requires periodic
updating.

Flow sensors
The detector uses flow sensors to monitor hydrogen flow. If the
Autoflow zero feature is on, they are zeroed automatically. This is
the recommended way. They can also be zeroed manually (see
“Zero a specific flow or pressure sensor” on page 44).

Pressure sensors
All EPC control modules use pressure sensors. The must be
zeroed individually. There is no automatic zero for pressure
sensors. Pressure sensors should be zeroed once every twelve
months.

Configure auto flow zero

A useful calibration option is Autoflow zero. When it is On, after
the end of a run the GC shuts down the flow of gases to an inlet,
waits for the flow to drop to zero, measures and stores the flow
sensor output, and turns the gas back on. This takes about two
seconds. The zero offset is used to correct future flow
measurements. Agilent recommends setting the detector to
automatically zero flow sensors to reduce drift.
To activate:
1 On the detector keypad, press [Options].
2 Scroll to Calibration and press [Enter].
3 Scroll to Autoflow zero (H2 Lower) and press [On/Yes]. (To turn
off autozero, instead press [Off/No].

Conditions for zeroing a sensor

Flow sensors are zeroed with the carrier gas connected and
flowing.
Pressure sensors are zeroed with the supply gas line
disconnected from the gas control module.

8355 S SCD and 8255 S NCD User Manual 43

4 Operation

Zero a specific flow or pressure sensor

1 Press [Options], scroll to Calibration, and press [Enter].
2 Scroll to the sensor to be zeroed and press [Enter].
3 Set the flow or pressure:
• Flow sensors. Verify that the gas is connected and flowing
(turned on).
• Pressure sensors. Disconnect the gas supply line at the
back of the GC. Turning it off is not adequate; the valve
may leak.
4 Scroll to the desired zero line.
5 Press [On/Yes] to zero or [Clear] to cancel.
6 Reconnect any gas line disconnected in step 3 and restore
operating flows.

44 8355 S SCD and 8255 S NCD User Manual

 Operation 4

Signal Output
The 8355 S and 8255 S detectors provides output data as an
analog signal. Analog output ranges are 0 to 1 V, 0 to 10 V, and
0 to 1 mV. To use the detector with Agilent GCs (6850, 6890,
7820, and 7890), an Analog to Digital converter, such as the
Agilent 35900E A/D Converter, or Analog Input Board (AIB) is
required.

6850 Series GCs

• A single channel detector can connect to an AIB (accessory
G3375A, or option 206), or external A/D converter.
• For a tandem FID/XCD, use an external A/D converter (such
as the 35900E).

6890 Series GCs

• A single channel detector can connect to an AIB (part
number G1556A, or option 206), or external A/D converter.
• A tandem configuration can use an AIB to collect the XCD
signal, but the 6890 only supports two detectors total. A
configuration such as dual FID-XCD, or an FID-XCD paired
with any other detector requires an external A/D converter
for the XCD.

7820 Series GCs

• Since an AIB is not supported by the 7820, you must use an
A/D converter to collect the XCD signal.

7890 Series GCs

• A single channel detector can connect to an AIB (accessory
G3456A, or option 206), or external A/D converter.

Intuvo 9000 GC
• A single channel detector can connect to an AIB
(accessory G3456A, or option 206), or external A/D
converter.

Signal Types
When assigning detector signals, use the [Mode/Type] and
choose from the Signal Type parameter list, or press a key or
combination of keys.

8355 S SCD and 8255 S NCD User Manual 45

4 Operation

The nondetector signal is test plot. Access the test plot by

pressing [Mode/Type]. Diagnostic signals are for use by your
service representative and are not described in detail here.

Value
Value on the sginal parameter list is the same as Detector on
the detector parameter list.

Analog Signals
If you use an analog recorder, you may need to adjust the signal
to make it more usable. Zero and Range in the signal parameter
list do this.

Analog zero
Zero subtracts value entered from baseline. Press [On/Yes] to
set to current Value or [Off/No] to cancel.
This is used to correct baseline elevation or offsets. A common
application is to correct a baseline shift that occurs as the result
of a valve operation. After zeroing, the analog output signal is
equal to the Value line of the parameter list minus the Zero
setpoint.
1 Verify that thew dectector is on and in a ready state.
2 Press [Analog Out].
3 Scroll to Zero.
4 Press [On/Yes] to set Zero at the current signal value, or
enter a number between -500000 and +500000. A value
smaller than the current Zero shifts baseline up.

Analog range
Range scales data coming from the detector.
Range is also referred to as gain, scaling, or sizing. It sizes the
data coming from the detector to the analog signal circuits to
avoid overloading the circuits (clamping). Range scales all
analog signals.
Valid setpoints are from 0 to 13 and represent 20 (=1) to 213
(=8192). Changing a setpoint by 1 changes the height of the
chromatogram by a factor of 2. The following chromatograms
illustrate this. Use the smallest possible value to minimize
integration error.

46 8355 S SCD and 8255 S NCD User Manual

 Operation 4

A: Range = 0 B: Range = 3 C: Range = 1

When developing a method, first set the analog range to 9, if

using an AIB, or to 10 if using an Agilent 35900E A to D. Adjust
as necessary to view your data.

Analog data rates

Your integrator or recorder must be fast enough to process data
coming from the GC. If it cannot keep up with the GC, the data
may be damaged. This usually shows up as broadened peaks
and loss of resolution.
Speed is measured in terms of bandwidth. Your recorder or
integrator should have a bandwidth twice that of the signal you
are measuring.

8355 S SCD and 8255 S NCD User Manual 47

4 Operation

Methods

To load a method
1 Press [Load].
2 Press [Method].
3 Enter the number of the method to be loaded.
4 Press [On/Yes] to load the method and replace the active
method. Alternatively, press [Off/No] to return to the stored
methods list without loading the method.

To store a method
1 Ensure that the proper parameters are set.
2 Press [Method].
3 Scroll to the method to store, then press [Enter].
4 Press [On/Yes] to store the method and replace the active
method. Alternatively, press [Off/No] to return to the stored
methods list without storing the method.

48 8355 S SCD and 8255 S NCD User Manual

 Operation 4

Resource Conservation
For optimal performance and precision, leave the detector at
operating conditions. The SCD achieves maximum precision
when maintained at operating conditions for a long period of
time. If your application requires the highest precision, you may
prefer to not use the resource conservation features with an
SCD. The NCD can more recover precision more quickly. With
either detector, consider the cost savings for the resources
against the recovery time for precision.

WA RNING Never put the detector into sleep mode while the GC is operating
normally.

Schedule
The detector uses a schedule, based on the on-board clock,
along with two special methods called SLEEP and WAKE. A
SLEEP method sets low flows and temperatures to conserve
resources. A WAKE method sets new flows and temperatures,
typically to restore operating conditions.
Load the sleep method at a specified time during the day to
reduce flows and temperatures. Load the wake method or
analytical method to restore settings before using the detector
again. For example, load the sleep method at the end of each
day or work week, then load the wake before arriving to work
the next day. Experiment to find the best time to load the wake
method.

Sleep Methods
Consider the following:
• Do not turn off the vacuum pump. The pump needs to be on
to prevent shutdown conditions.
• Do not turn off the oxidizer flow.
• To conserve oxygen, turn off the ozone generator. This setting
also turns off the oxygen flow.
For SCD:
The main concern is to avoid heating the ceramic tube without
all gases flowing. Turning off the ozone generator will conserve
oxygen without changing the flows through the ceramic tube. If
you must reduce temperature or gas flow further, then you can

8355 S SCD and 8255 S NCD User Manual 49

4 Operation

reduce the oxidizer flow, turn off the hydrogen flows, and most
importantly, reduce the burner temperature to about 250 C. The
base temperature can be reduced also.
For NCD:
Turn off the ozone generator. If needed to further conserve
energy and gases, reduce (but do not turn off) the oxygen and
turn off the hydrogen flow. Reduce the burner temperature to
about 250 °C and turn off the chiller.

To Set the Detector to Conserve Resources

Set the detector to conserve resources by selecting and using an
Instrument Schedule:
1 Decide how to restore flows. The choices from the Schedule
Function are:
• Go to Sleep with SLEEP method. This method should
reduce flows and temperatures. (While it is good practice
to create these methods, you do not need them if you only
wake the detector to the last active method.)
• Wake with the current method. At the specified time, the
detector will restore the last active method used before it
went to sleep.
• Wake with WAKE method. At the specified time, the
detector will load the wake method, and remain at those
settings.
2 Create a SLEEP method. This method should reduce flows
and temperatures.
3 Program the WAKE method, as needed. (While it is good
practice to create these methods, you do not need them if you
only wake the detector to the last active method.)
4 Create the Sleep/Wake Schedule.
a Press [Sleep/Wake].
b Scroll to Edit the Instrument Schedule? and press [Enter].
c Press [Mode/Type] to create a new schedule item.
d When prompted, scroll to the desired day of the week and
press [Enter].
e When prompted, scroll to Go to Sleep with SLEEP
method and press [Enter] then input the event time. Press
[Enter]

50 8355 S SCD and 8255 S NCD User Manual

 Operation 4

f If desired, set the wake function while still viewing the

schedule. Press [Mode/Type] to create a new schedule
item.
g When prompted scroll to the desired day of the week and
press [Enter].
h When prompted, scroll to Wake with the current method
or Wake to Wake method and press [Enter], then input the
event time. Press [Enter]
i Repeat steps b through g as needed for any other days of
the week.
You do not have to program events for every day. For example,
you can program the detector to sleep on Friday evening, then
wake on Monday morning, keeping it continuously at operating
conditions during weekdays.

To create or edit an instrument schedule

To create a new schedule or edit an existing schedule, delete
unwanted items, then add new items as desired.
1 Create the Sleep/Wake Schedule:
a Press [Sleep/Wake].
b Scroll to Edit the Instrument Schedule? and press [Enter].
c Press [Mode/Type] to create a new schedule item.
d When prompted, scroll to the desired day of the week and
press [Enter].
e When prompted, scroll to Go to Sleep with SLEEP
method and press [Enter] then input the event time. Press
[Enter]
f If desired, set the wake function while still viewing the
schedule. Press [Mode/Type] to create a new schedule
item.
g When prompted scroll to the desired day of the week and
press [Enter].
h When prompted, scroll to Wake with the current method
or Wake to Wake method and press [Enter], then input the
event time. Press [Enter]
i Repeat steps b through g as needed for any other days of
the week.

8355 S SCD and 8255 S NCD User Manual 51

4 Operation

2 Edit the Sleep/Wake Schedule:

a Load a method with similar setpoints.
b Edit the method setpoints. The detector only allows for
setting relevant parameters.
• For a SLEEP method, the detector sets the initial detector
temperature and flow rates.
• For a WAKE method, the detector sets the same
parameters as the sleep method.
c Press [Method], scroll to the method to store (SLEEP or
WAKE), and press [Store]. press [Enter].
d If prompted to overwrite, press [On/Yes] to overwrite the
existing method or [Off/No] to cancel.

To put the detector to sleep now

1 Press [Sleep/Wake].
2 Select Go to sleep now, then press [Enter].

To wake the detector now

1 Press [Sleep/Wake].
2 Select the desired wake choice, then press [Enter].
• When prompted, scroll to Wake with the current method
and press [Enter]. Exit sleep mode by loading the last
active method used before going to sleep.
• Wake to Wake method and press [Enter]. Exit sleep mode
by loading the WAKE method.

52 8355 S SCD and 8255 S NCD User Manual

Agilent 8355 S SCD and 8255 S NCD Detectors
User Manual

5
Maintenance

Maintenance Schedule 54
Tracking Detector Sensitivity 55
Consumables and Replacement Parts 56
Exploded Parts View of the SCD 58
Exploded Parts View of the NCD 59
Detector Maintenance Method 60
Attach a Column to the Detector 61
Replace the Inner Ceramic Tube (SCD) 64
Replace the Quartz Tube (NCD) 67
Check the Vacuum Pump Oil 71
Add Vacuum Pump Oil 72
Replace the Vacuum Pump Oil 74
Replace the Ozone Trap 76
Change the Oil Mist Filter 77
Clean the Detector Exterior 78
Calibrate the Flow and Pressure Sensors 79

This chapter describes the routine maintenance procedures

needed for normal use of the SCD and NCD.

Agilent Technologies 53
5 Maintenance

Maintenance Schedule
To maintain optimum performance of the Agilent 8355 S SCD
and 8255 S NCD, routinely replace the ozone trap, oil coalescing
filter, and vacuum pump oil. Refer to Table 3 for the expected
life span of each item.

Table 3 Recommended Edwards RV5 vacuum pump maintenance

schedule

Component Operating life*

Ozone destruction trap (converts O3 to O2) ~ 6 months
Oil coalescing filter ~ 3 months
Oil odor filter ~ 3 months if needed
Pump oil† ~ 3 months
Oil level Check weekly
*
The operating life is based on the total time logged during operation of the detector with
the burner and the ozone generator On.
†
Pump oil can be purchased from a supplier or directly from Agilent: SAE 10W-30,
Multiviscosity Synthetic Motor Oil such as, MOBIL 1 or AMSOIL.

54 8355 S SCD and 8255 S NCD User Manual

 Maintenance 5

Tracking Detector Sensitivity

Sensitivity reflects the performance characteristics of a given
system, and decreased sensitivity may indicate the need for
routine detector maintenance.
The MDL specifications are defined using the Agilent checkout
standard for SCD or NCD.
Sensitivity is typically reported as:

peak area
Sensitivity =
amount

Calculate a minimum detection limit (MDL) from the following

formula:

2 x noise
MDL =
sensitivity

where the noise is the ASTM noise reported by the Agilent data
system.

8355 S SCD and 8255 S NCD User Manual 55

5 Maintenance

Consumables and Replacement Parts

See the Agilent catalog for consumables and supplies for a more
complete listing, or visit the Agilent Web site for the latest
information (http://www.chem.agilent.com/store).

Table 4 Consumables and parts for the SCD and NCD

Description/quantity Part number

Detector parts
Ceramic tube, inner, small (SCD) (pack of 3) G3488-60008
(See Exploded Parts View of the SCD)
Quartz tube (NCD) G6600-80063
Ferrule, 1/4-inch, graphite, straight, 10/pk for SCD 0100-1324
outer ceramic tube and NCD quartz tube
Column installation tool  G3488-81302
(See Exploded Parts View of the SCD)
Sulfur chemiluminescence test sample 5190-7003
Nitrogen chemiluminescence test sample 5190-7002
Vacuum pump parts
RV5 pump – 110 V/230 V – Inland G6600-64042
Pump tray, RV5 pump G1946-00034
PM Kit, RV5 oil pump G6600-67007
Oil mist filter for RV5 pump, for SCD/NCD G6600-80043
Replacement oil coalescing filter, RV5 pump G6600-80044
Replacement odor filtration element G6600-80045
Ozone destruction trap G6600-85000
Oil return line, RV5 pump 3162-1057
Oil, synthetic, Mobil 1 G6600-85001
NW 20/25 clamping ring (for oil mist filter) 0100-0549
NW 20/25 clamping ring (for exhaust hose) 0100-1398
Tools
Funnel 9301-6461
Wrench, Allen, 5-mm 8710-1838
Screwdriver, flat-bladed 8710-1020
Gloves, chemical resistant, lint-free 9300-1751

56 8355 S SCD and 8255 S NCD User Manual

 Maintenance 5

Table 5 Filters for the SCD and NCD

Description/quantity Part number

Gas Clean filter, sulfur (filters sulfur and moisture) CP17989
Gas Clean Filter SCD Kit, for sulfur CP17990
chemiluminescence detectors

Table 6 Nuts, ferrules, and hardware for capillary columns

Column id (mm) Description Typical use Part number/quantity

.53 Ferrule, graphite, 1.0-mm id 0.53-mm capillary columns 5080-8773 (10/pk)
Ferrule, graphite, 0.8-mm id 0.53-mm capillary columns 500-2118 (10/pk)
Column nut, finger-tight (for Connect column to inlet or detector 5020-8293
0.53-mm columns)
.45 Ferrule, graphite, 0.8-mm id 0.45-mm capillary columns 500-2118 (10/pk)
.32 Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 0.25-mm, and 5080-8853 (10/pk)
0.32-mm capillary columns
Column nut, finger-tight Connect column to inlet or detector 5020-8292
(for .100- to .320-mm columns)
.1 – .25 Ferrule, graphite, 0.4-mm id 0.1-mm, 0.2-mm, 0.25-mm, and 500-2114 (10/pk)
0.32-mm capillary columns
Column nut, finger-tight (for Connect column to inlet or detector 5020-8292
.100- to .320-mm columns)
All Ferrule, no-hole Testing 5181-3308 (10/pk)
Capillary column blanking nut Testing–use with any ferrule 5020-8294
Column nut, universal Connect column to inlet or detector 5181-8830 (2/pk)
Column cutter, ceramic wafer Cutting capillary columns 5181-8836 (4/pk)
Ferrule tool kit Ferrule installation 440-1000

8355 S SCD and 8255 S NCD User Manual 57

5 Maintenance

Exploded Parts View of the SCD

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2XWOHWÀWWLQJ
6ZDJHORNQXW
8SSHUÀWWLQJ
25LQJ
LQFK6WDLQOHVVVWHHO
WXELQJXSSHUK\GURJHQ

,QQHUFHUDPLFWXEH
6ZDJHORNQXW66LQFK

6KURXGDVVHPEO\ LQFKJUDSKLWHIHUUXOHVWUDLJKW

2XWHUFHUDPLFWXEH

%XUQHUKHDWHU

%XUQHUORZHUQXW

LQFKJUDSKLWHIHUUXOHVWUDLJKW
-HWDVVHPEO\DQGFRXSOLQJ

'HWHFWRUEDVH

,QVXODWLRQWRS
,QVXODWLRQERWWRP (For tandem FID-SCD, see the
FID details)
,QVXODWLRQFXS
)HUUXOHFROXPQ

&ROXPQQXW

&ROXPQLQVWDOODWLRQWRRO

Figure 8 SCD Exploded parts view

58 8355 S SCD and 8255 S NCD User Manual

 Maintenance 5

Exploded Parts View of the NCD

Coupling

1/4-inch graphite ferrule, straight

Quartz tube
Shroud assembly

Burner heater

Burner lower nut

1/4-inch graphite ferrule, straight
Jet assembly and coupling

Detector base

Insulation, top

Insulation, bottom

Insulation cup

Ferrule
Column nut

Column installation tool

Figure 9 NCD exploded parts view

8355 S SCD and 8255 S NCD User Manual 59

5 Maintenance

Detector Maintenance Method

It is good practice to create a maintenance method for the GC
that prepares the GC and detector for maintenance. Load this
method before performing maintenance.
A maintenance method for the SCD or NCD should do the
following:
1 Turn off the heater and burner to allow them to cool.
2 Turn off all hydrogen flows.
3 Leave on the oxidizer and ozone generator supply gases.
4 Turn off the ozone generator.
5 Leave on the vacuum pump.
6 Keep (helium) carrier gas flowing.
7 Set the oven to 30 °C to minimize column bleed.

In addition, cool any other parts of the detector as needed.

Allow heated zones to cool to < 40 °C for safe handling.

60 8355 S SCD and 8255 S NCD User Manual

 Maintenance 5

Attach a Column to the Detector

(Does not apply to the Intuvo 9000 GC.)

This procedure describes how to attach a column directly to an XCD. In a

NOTE
tandem FID-XCD installation, install the column into the FID as described
in the FID instructions. See the GC documentation.

1 Gather the following materials (see “Consumables and parts

for the SCD and NCD” on page 56):
• Column installation tool for SCD/NCD (G3488-81302)
• Column
• Ferrule (for column)
• Column nut
• Column cutter
• 1/4-inch open-end wrench
• Septum
• Isopropanol
• Lab tissue
• Lint-free gloves
• Magnifying loupe

WA RNING The oven, inlet, or detector may be hot enough to cause burns. If
the oven, inlet, or detector is hot, wear heat-resistant gloves to
protect your hands.

WA RNING Wear safety glasses to protect your eyes from flying particles
while handling, cutting, or installing glass or fused silica
capillary columns. Use care in handling these columns to prevent
puncture wounds.

CAUTION Wear clean, lint-free gloves to prevent contamination of parts with

dirt and skin oils.

8355 S SCD and 8255 S NCD User Manual 61

5 Maintenance

2 Cool the GC oven, inlet, and other heated zones to a safe

handling temperature (< 40 °C).
3 Prepare the detector for maintenance.
a Load the maintenance method and wait for the detector to
become ready. (See “Detector Maintenance Method” on
page 60.) Wait until the detectors, burner assembly, and
detector base cool to a safe handling temperature
(< 40 °C).
b Turn off all hydrogen flows. (Leave on the oxidizer and
ozone supply gases.)
c Turn off the ozone generator.

WA RNING Hydrogen gas is flammable. Turn off all detector (and column)
hydrogen gas flows before performing maintenance on the
detector.

4 Place a septum, capillary column nut, and ferrule on the

column.

Column nut Ferrule Column

Septum

Figure 10 Place septum, column nut, and ferrule on the column

62 8355 S SCD and 8255 S NCD User Manual

 Maintenance 5

5 Insert the end of the column through the column measuring

tool so that the end protrudes beyond the tool.

Score column here

Column measuring tool

Column nut
78 ± 1 mm
Ferrule

Figure 11 Set column length and swage ferrule using column measuring tool

6 Tighten the column nut into the column measuring tool until
the column nut grips the column. Tighten the nut an
additional 1/8- to 1/4-turn with a pair of wrenches. Snug the
septum against the base of the column nut.
7 Use a column cutting wafer at 45° to score the column.
8 Snap off the column end. The column may protrude about
1 mm beyond the end of the tool. Inspect the end with a
magnifying loupe to make certain that there are no burrs or
jagged edges.

Bad

Good
9 Remove the column, nut, and swaged ferrule from the tool.
10 Wipe the column walls with a tissue dampened with
isopropanol to remove fingerprints and dust.
11 Carefully thread the swaged column into the detector fitting.
Finger-tighten the column nut, then use a wrench to tighten
an additional 1/8 turn.

8355 S SCD and 8255 S NCD User Manual 63

5 Maintenance

Replace the Inner Ceramic Tube (SCD)

To replace the inner ceramic tube:

WA RNING The oven, inlets, and detectors can be hot enough to cause burns.
Cool these areas to a safe handling temperature before beginning.

CAUTION Wear clean, lint-free gloves to prevent contamination of parts with

dirt and skin oils.

CAUTION Most steps in this procedure require the use of two wrenches, one
to hold the burner steady and the other to loosen a part. Always use
two wrenches to avoid over-torquing or bending the burner
assembly.

1 Gather the following:

• Two 7/16-inch open-end wrenches
• 3/8-inch open-end wrench
• New O-ring
• New ceramic tube
• Tweezers
• 1/8-inch cap for transfer line
• T20 Torx driver
2 Cool the GC oven, inlet, and other heated zones to a safe
handling temperature (< 40 °C).
3 Prepare the detector for maintenance.
a Load the maintenance method and wait for the detector to
become ready. (See “Detector Maintenance Method” on
page 60.) Wait until the detectors, burner assembly, and
detector base cool to a safe handling temperature
(< 40 °C).
b Turn off all hydrogen flows. (Leave on the oxidizer and
ozone supply gases.)
c Turn off the ozone generator.

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 Maintenance 5

WA RNING Hydrogen gas is flammable. Turn off all detector (and column)
hydrogen gas flows before performing maintenance on the
detector.

4 Disconnect the transfer line and quickly cover the open end
with the 1/8-inch cap. Use a 3/8-inch wrench on the transfer
line and a 7/16-inch wrench on the upper fitting to hold the
burner assembly steady.
5 Using two 7/16-inch wrenches, remove the outlet fitting from
the upper fitting.
6 If the old O-ring is stuck to the bottom of the outlet fitting,
use tweezers or similar to gently pry it loose from the fitting.
7 Remove the old inner ceramic tube.
8 Place a new O-ring over the end of the new inner ceramic
tube, and slide the O-ring about 7 mm down the tube. (This
dimension is not critical.)

Inner ceramic tube O-Ring

~ 7 mm
9 Gently insert the tube and O-ring assembly into the burner
until it rests on the O-ring.
10 Orient the outlet fitting so the hex flats are closer to the
upper fitting, as shown, and install over the ceramic tube.
Tightening the outlet fitting will automatically adjust the
O-ring and ceramic tube positions. Tighten until snug
(finger-tight). Do not overtighten.

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5 Maintenance

11 Reinstall the transfer line onto the outlet fitting. Tighten

until snug (finger-tight). Do not overtighten.
12 Restore the detector gas flows.
13 Check for leaks at the upper hydrogen fitting. Correct a leak
as needed.
14 Restore the remaining detector operating conditions.

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 Maintenance 5

Replace the Quartz Tube (NCD)

To replace the NCD quartz tube:

WA RNING The oven, inlets, and detectors can be hot enough to cause burns.
Cool these areas to a safe handling temperature before beginning.

CAUTION Wear clean, lint-free gloves to prevent contamination of parts with

dirt and skin oils.

CAUTION Most steps in this procedure require the use of two wrenches, one
to hold the burner steady and the other to loosen a part. Always use
two wrenches to avoid over-torquing or bending the burner
assembly.

1 Gather the following:

• Two 7/16-inch open-end wrenches
• 3/8-inch open-end wrench
• 5/8-inch open-end wrench
• New quartz tube
• Tweezers
• 1/8-inch cap for transfer line
• T20 Torx driver
• Dental tool or similar tool for graphite ferrule removal
• 2 New graphite ferrules
2 Cool the GC oven, inlet, and other heated zones to a safe
handling temperature (< 40 °C).
3 Prepare the detector for maintenance.
a Load the GC maintenance method and wait for the GC to
become ready. (See “Detector Maintenance Method” on
page 60.) Wait until the detectors, burner assembly, and
detector base cool to a safe handling temperature
(< 40 °C).
b Turn off all hydrogen flows. (Leave on the oxidizer and
ozone supply gases.)

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5 Maintenance

c Turn off the ozone generator.

WA RNING Hydrogen gas is flammable. Turn off all detector (and column)
hydrogen gas flows before performing maintenance on the
detector.

4 Remove the protective shroud. Remove the two T20 Torx

screws, twist the shroud counter-clockwise to remove it from
the mounting posts, then lift. Set the shroud and screws
aside for later use.
5 Disconnect the transfer line and quickly cover the open end
with the 1/8-inch cap. Use a 3/8-inch wrench on the transfer
line and a 7/16-inch wrench of the upper fitting to hold the
burner assembly steady.
6 Using two 7/16-inch wrenches, remove the outlet fitting from
the nut on the top of the quartz tube.
7 Gently slide the nut and its ferrule up and off of the quartz
tube.

CAUTION The quartz tube is fragile and can be chipped or cracked. To avoid
damaging the quartz tubes, handle carefully.

8 Using 5/8-inch and 9/16-inch wrenches, remove the burner

assembly and tube from the coupling in the detector base
assembly.
9 Inspect the area around the jet in the coupling. If there are
broken bits of tube present, remove with tweezers or similar
tool.

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 Maintenance 5

10 Gently pull the quartz tube up through the burner assembly

to remove. The graphite ferrule should remain in the rotating
nut in the burner base.
11 Use a dental tool or similar to remove the old graphite
ferrule from the rotating nut in the burner base.
12 Use two wrenches to disassemble the reducer, then remove
the old ferrule.
13 Install new graphite ferrules. In both cases, the tapered end
of the ferrule faces out, away from the burner.

Reducer, top

Ferrule Rotating lower nut

Ferrule
Reducer, bottom

Quartz tube

14 Reassemble the reducer. Tighten with two wrenches until

snug.
15 Slide the new quartz tube down through the burner assembly
until it protrudes from the base about 1 cm. (This dimension
is not critical. The tube position will adjust as you tighten the
lower nut onto the coupling.)

CAUTION When tightening the graphite ferrules onto a quartz tube, tighten
only until snug. Over tightening can damage the ferrules or quartz
tubes.

16 Carefully lower the burner assembly onto the detector base

and thread the nut onto the detector base assembly by hand.
Tighten finger-tight, then snug in place using a wrench. Do
not overtighten.
17 Place the nut and ferrule over the open end of the quartz
tube so that the open end of the nut faces up.
18 Install the nut into the outlet fitting and tighten with two
wrenches just until snug.
19 Reinstall the transfer line onto the outlet fitting. Tighten
until snug (finger-tight). Do not overtighten.

8355 S SCD and 8255 S NCD User Manual 69

5 Maintenance

20 Reinstall the protective shroud.

21 Restore the detector operating conditions.

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 Maintenance 5

Check the Vacuum Pump Oil

CAUTION Never add or replace the foreline pump oil while the pump is on.

Check the level and color of the pump oil weekly.

1 Check the oil level in the window of the foreline pump. The
oil level should be between the marks for Max and Min.

Max

Oil level

Min

Figure 12 Checking the oil level

2 Check that the color of the pump oil is clear or almost clear
with few suspended particles. If the pump oil is dark or full
of suspended particles, replace it.
3 Record the maintenance in the maintenance logbook.

8355 S SCD and 8255 S NCD User Manual 71

5 Maintenance

Add Vacuum Pump Oil

Add pump oil when the pump oil level is low.
Materials needed
• Funnel (9301-6461)
• 5-mm Allen wrench (8710-1838)
• Gloves, chemical resistant, clean, lint free (9300-1751)
• Oil, synthetic, Mobile 1 (G6600-85001)
• Safety glasses (goggles)

WA RNING Never add pump oil while the pump is on.

WA RNING The fill cap and pump may be dangerously hot. Check that the fill
cup and pump are cool before you touch them.

CAUTION Use only synthetic 10W30 oil, such as Mobil 1. Any other oil can
substantially reduce pump life and invalidates the pump warranty.

Procedure
1 Shut down the detector and wait for the pump to turn off.
See “Shutdown” on page 42.
2 Turn off the detector and unplug the pump power cord at the
pump.

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 Maintenance 5

3 Remove the fill cap on the vacuum pump.

Power cord
Fill cap receptacle

9ROWDJHFRQÀJXUDWLRQ
SOXJ

4 Add new pump oil until the oil level is near, but not over the
maximum mark beside the oil level window. See Figure 12 on
page 71.
5 Reinstall the fill cap.
6 Wipe off all excess oil around and underneath the pump.
7 Reconnect the pump power cord.
8 Turn on the detector and restore operating conditions. See
“Start-up” on page 41.
9 Record the maintenance in the maintenance logbook.

8355 S SCD and 8255 S NCD User Manual 73

5 Maintenance

Replace the Vacuum Pump Oil

Replace the pump oil every three months or sooner if the oil
appears dark or cloudy.
Materials needed
• Container for catching used pump oil
• Funnel (9301-6461), 5-mm Allen wrench (8710-1838)
• Gloves, chemical resistant, clean, lint free (9300-1751)
• Oil, synthetic, Mobile 1 (G6600-85001)
• Safety glasses (goggles)
• Screwdriver, flat-bladed, large (8710-1029)

WA RNING Never add pump oil while the pump is on.

WA RNING The fill cap and pump may be dangerously hot. Check that the fill
cup and pump are cool before you touch them.

WA RNING Do not touch the oil. The residues from some samples are toxic.
Properly dispose of the oil.

CAUTION Use only synthetic 10W30 oil, such as Mobil 1. Any other oil can
substantially reduce pump life and invalidates the pump warranty.

Procedure
1 Shut down the detector and wait for the pump to turn off.
See “Shutdown” on page 42.
2 Turn off the detector and unplug the pump power cord at the
pump.

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 Maintenance 5

3 Place a container under the drain plug of the vacuum pump.

Fill cap

Drain plug

4 Remove the fill cap, then open the drain plug. Drain the oil
completely by raising the motor end of the pump.
5 Reinstall the drain plug.
6 Add new pump oil until the oil level is near, but not over the
maximum mark beside the oil level window. See Figure 12 on
page 71.
7 Reinstall the fill cap.
8 Wipe off all excess oil around and underneath the pump.
9 Reconnect the pump power cord.
10 Turn on the detector and restore operating conditions. See
“Start-up” on page 41.
11 Record the maintenance in the maintenance logbook.
12 Check the pump for leaks after about 30 minutes, and check
again after 24 hours.

8355 S SCD and 8255 S NCD User Manual 75

5 Maintenance

Replace the Ozone Trap

To replace the ozone trap:
1 Load a method to cool the detector, turn off the heaters, and
turn off the hydrogen flow.
• Turn off the heaters and allow the burner to cool.
• Leave the oxidizer flow on.
• Turn off the hydrogen flow.
• Turn off the vacuum pump.
• Set the GC oven to 30 °C (or off) to minimize column
bleed.
• Leave (helium) carrier gas flowing.
2 Allow the vacuum pump to cool to a safe handling
temperature.
3 Remove the trap assembly and vacuum hose from the
support bracket.
4 Loosen the two hose clamps that secure the old ozone trap in
place.
Hose clamp
Ozone trap

Hose clamp

5 Remove the trap from the pump intake hose. (If needed,
loosen the clamp at the pump intake.)
6 Lift the old trap from the support bracket, then remove the
detector vacuum hose from the barbed fitting on the old trap.
7 Install the new trap. Make sure that the flow direction arrow
on the new trap points towards the intake fitting. (The trap
elbow must be nearest the pump intake.) If you removed the
short connector hose from the pump intake, reinstall it.

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 Maintenance 5

Change the Oil Mist Filter

The oil mist filter on the RV5 pump has two components: the
charcoal odor filter and the oil coalescing filter element. To
replace the filters, disassemble the oil mist filter assembly with
the 4 mm long-handled hex wrench (provided). The smaller
charcoal odor filter sits on top of the larger oil coalescing filter
element. While it is recommended to replace the oil coalescing
filter element after 90 days of continuous use, replacement of
the charcoal odor filter is optional. After replacing the filter,
re-assemble the filter assembly and attach it to the pump flange.

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5 Maintenance

Clean the Detector Exterior

WA RNING Burn hazard. The burner assembly can be hot enough to cause
burns. Before touching, cool to a safe handling temperature
(< 40 °C).

WA RNING Shock hazard. Before cleaning the detector, turn it off and unplug
its power cord.

Before cleaning the detector, shut it down, turn it off, and

unplug the detector power cord. Clean the detector with a damp
cloth using water. Do not spray liquids directly onto the
detector. Wipe dry with a clean, soft cloth. Do not allow cleaning
fluids to drip into the detector or GC because liquids can
damage the detector or GC electronics.
Do not use cleaning agents on the burner assembly that could
cause a hazard on the burner.

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 Maintenance 5

Calibrate the Flow and Pressure Sensors

The 8355 S SCD and 8255 S NCD use electronic pressure control
modules. Typically, set the detector to use automatic flow
zeroing. See “Configure auto flow zero” on page 43. Calibration
is generally not required. However, if needed the flow and
pressure sensors can be manually zeroed. See “Zero a specific
flow or pressure sensor” on page 44 for details.

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5 Maintenance

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Agilent 8355 S SCD and 8255 S NCD
User Manual

6
Troubleshooting
Solving Detector Problems 82
Troubleshooting Table 83
Status Indicator LED 86
Detector Messages 87
Leaks 88
Power Problems 90
Ozone Generation Problems 91
Coking 92
Hydrogen Poisoning 93
Contaminated Gases 94

This chapter describes how to troubleshoot and resolve typical

issues encountered while using an Agilent 8355 S SCD or 8255 S
NCD detector.

Agilent Technologies 81
6 Troubleshooting

Solving Detector Problems

A basic understanding of the detector helps to diagnose and
solve detector problems. Review the basic detector theory found
in “Theory of Operation” on page 18. Also, please note that this
section is intended to troubleshoot problems in a detector that
has previously been performing acceptably. If trying to optimize
a new detector application, see “Adjusting the Operating
Conditions” on page 40 for recommendations on adjusting
method setpoints to obtain better results.
Many symptoms may be caused by more than one problem or by
poor chromatographic technique. Analysis of sulfur or nitrogen
compounds has traditionally been very difficult because of the
inherent reactivity and instability of the compounds
themselves. Often, problems initially blamed on the detector
actually originate from either poor chromatographic technique
or other system failures (for example, a leak at the column inlet
fitting). Therefore, the first step in troubleshooting is to isolate
the problem to the GC (inlet, injector, or column), to the burner
assembly, or to the detector (ozone generator, vacuum pump,
photomultiplier tube, or electronics). When diagnosing a
problem in a system that had been working, a good first step is
to restore the default typical operating conditions. The response
under these conditions can help determine whether or not the
method settings are causing the problem.
Table 7 in the next section lists many common problems, their
most probable causes, and corrective action that should be
taken.

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 Troubleshooting 6

Troubleshooting Table

Table 7 Troubleshooting Detector Issues

Problem Possible cause Diagnosis Corrective action

Detector problems
No response No ozone Little or no difference in See “No ozone”.
output signal between ozone
On and Off.
Incorrect range setting for Edit the range to better scale
analog out (standalone the data. See “Signal
detector only) Output” on page 45.
No ozone High voltage transformer No difference in output Contact Agilent for service.
and/or ozone generator signal between ozone On See “The Service Mode Key”
inoperative. and Off even though flow on page 32.
through the ozone generator
is normal.
Restriction in ozone supply Contact Agilent for service.
to the reactor cell.
No Response Broken ceramic or quartz Replace the ceramic tube.
tube. See “Replace the Inner
Ceramic Tube (SCD)” on
page 64 or “Replace the
Quartz Tube (NCD)” on
page 67.
Low Response Inappropriate hydrogen and Check flow rates. Adjust flow rates.
oxidizer flow rates.
Leak in the detector. Check for leaks in the
detector and repair any
leaks. See “Leaks” on
page 88.
Contaminated ceramic or If there does not appear to Replace the ceramic tube.
quartz tubes. be a leak, then inspect the See “Replace the Inner
ceramic tube. Contamination Ceramic Tube (SCD)” on
can result from column page 64 or “Replace the
bleed, samples which Quartz Tube (NCD)” on
contain volatile metal page 67.
complexes, and large
injections of coke-forming
hydrocarbons.
Input voltage does not Contact Agilent for service.
match configuration plug.

8355 S SCD and 8255 S NCD User Manual 83

6 Troubleshooting

Table 7 Troubleshooting Detector Issues

Problem Possible cause Diagnosis Corrective action

Wandering Baseline Contamination in one of the Check the difference in the Check inline supply traps
detector gases. output signal between ozone and replace.
On and Off. Change detector gases.
Excessive response Incorrect range setting for Edit the range to better scale
analog out (standalone the data. See “Signal
detector only) Output” on page 45.
Leak in the oxidizer lines. Check for leaks in the
detector and repair any
leaks. See “Leaks” on
page 88.
Leak in the hydrogen supply Check for leaks in the
lines. detector and repair any
leaks. See “Leaks” on
page 88.
Tailing peaks with Severe contamination of High background signal Check inline supply traps
non-equimolar response detector gases. compared against ozone Off. and replace.
Change detector gases.
Tailing peaks Poor column connection. Verify column position at Reinstall column. See
inlet and outlet. Look for “Attach a Column to the
discoloration of column at Detector” on page 61.
detector fitting which
indicates column in
combustion zone.
Cracked tubes. Confirm pressure and Replace the ceramic tube.
vacuum ranges. Inspect See “Replace the Inner
columns and ferrules. Ceramic Tube (SCD)” on
page 64 or “Replace the
Quartz Tube (NCD)” on
page 67.
Detector thermal shutdown Thermocouple open. Contact Agilent for service.
Burner pressure exceeds Restriction caused by upper If performing maintenance,
760 Torr. ceramic tube inner diameter. complete it. Recheck again
during normal operation.
Burner pressure excessively Cracked quartz or outer Replace the ceramic tube.
high. ceramic tube. See “Replace the Inner
Leaking or disconnected Ceramic Tube (SCD)” on
1/16-inch stainless steel page 64 or “Replace the
hydrogen or oxidizer line. Quartz Tube (NCD)” on
page 67.
Check connection. Check
line for leaks. Contact
Agilent for service if the line
is cracked.

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 Troubleshooting 6

Table 7 Troubleshooting Detector Issues

Problem Possible cause Diagnosis Corrective action

Leak in burner. Check for leaks in the
detector and repair any
leaks. See “Leaks” on
page 88.
Burner pressure lower than Cracked or misaligned inner Check that the inner ceramic See “Replace the Inner
expected and poor response ceramic tube. tube is positioned correctly Ceramic Tube (SCD)” on
and has not dropped down page 64.
into the outer tube.

Table 8 Troubleshooting Pump Issues

Problem Possible Cause Diagnosis Corrective Action

Vacuum pump problems
Pump does not start Pump switch off or power Turn On pump power switch.
cord disconnected. Check pump power cord.
Fuses blow on startup Emulsified oil. Inspect oil for integrity. Change pump oil, and plug
unit into wall to run for
10–15 minutes.
Contact Agilent to replace
blown fuses.
Water in pump Cracked coalescing filter. Milky yellow oil in the pump Change coalescing filter and
window. pump oil.
Reaction cell pressure high Ozone destruction trap Remove ozone destruction Change chemical trap.
clogged. trap from the vacuum line
and re-check expected
pressure readings.
Burner disconnected from Check connections.
reaction cell.
Vacuum pump defective. Replace vacuum pump.
Pump loses oil gurgle sound Ballast open. Oil level drops. Reset ballast. See
pump-specific sections.
High level of oil in Plugged oil return restrictor. No visible movement of oil Change filter and clear
coalescing filter in the return line. restrictor.

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6 Troubleshooting

Status Indicator LED

Use the detector status LED to quickly determine the status and
readiness of the detector. The LED changes color depending on
the current state of the detector.
• Green: Indicates that power is available for the heaters,
chiller (NCD), vacuum pump, and ozone generator.
• Yellow: Indicates that the detector is not ready for operation.
Power is on and available, but not all parameters have
reached operating setpoints. A warning or other message
may exist.
• Red: Indicates a fault or other serious condition. A fault or
other message may exist. The detector cannot be used until
the fault condition is resolved.

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 Troubleshooting 6

Detector Messages
Check the detector status display for detector messages. The
detector keypad will display and status and error messages that
occur during operation, as well as log detector maintenance and
error messages in the detector log files.

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6 Troubleshooting

Leaks

Ozone leaks

WA RNING Ozone is a hazardous gas and a strong oxidant. Exposure to ozone

should be minimized by using the instrument in a well-ventilated
area and by venting the exhaust of the vacuum pump to a fume
hood. The ozone generator should be turned off when the
instrument is not in use.

If you suspect an ozone leak, shut down the detector. Do not

open the detector mainframe. Contact Agilent for service.

Hydrogen leaks

WA RNING Do not measure hydrogen together with air or oxygen. This can
create explosive mixtures that may be ignited by the high burner
temperature. To avoid this hazard: 1. Cool the burner before you
begin. 2. Always measure gases separately.

Check all external connections for leaks. See “Checking for

hydrogen and oxidizer leaks” on page 89. Check the supply
connections to the detector mainframe and between the
detector mainframe and the burner assembly. If you suspect a
leak inside the detector mainframe, contact Agilent for service.
Do not open the detector mainframe.

Oxidizer leaks

WA RNING Oxygen rich environments can promote combustion and even

result in spontaneous combustion under conditions of high
pressure and exposure to contamination. Use only oxygen rated
components and ensure that components are oxygen clean prior
to use with pure oxygen.

Check the oxidizer supply connections to the detector

mainframe and between the detector mainframe and the burner
assembly. See “Checking for hydrogen and oxidizer leaks” on

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 Troubleshooting 6

page 89. If you suspect a leak inside the detector mainframe,

contact Agilent for service. Do not open the detector
mainframe.

Checking for hydrogen and oxidizer leaks

To check for a leak in the hydrogen or oxidizer flow paths, do
the following:
1 Check all external fittings for leaks. Correct any leaks
(tighten or remake connections as appropriate).
2 If you still suspect a leak, establish the typical flow checkout
conditions (see Table 10 on page 100 for SCD or Table 11 on
page 106 for NCD).
3 Maintain these conditions for several minutes. If the detector
cannot maintain these flow rates, contact Agilent for service.
4 If the detector was able to maintain the flow rates, turn off
all gas flows using the detector keypad.
5 Monitor the pressure readings on the detector display. (Press
[Det].) With the vacuum pump running, the reaction cell
pressure should fall to approximately 0 (zero). The burner
pressure should fall to a value considerably lower than the
typical operating pressure. This process will take time due to
the internal configuration of the burner assembly. If the
burner pressure remains high or at normal pressures,
contact Agilent for service.

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6 Troubleshooting

Power Problems
The power supplied to the SCD/NCD heaters, NCD chiller,
vacuum pump, and ozone generator comes from the detector
mainframe and is controlled by the detector power switch.

No power
If the detector does not appear to have power—if the vacuum
pump does not run and the heaters will not turn on—check the
following:
• Check that the power switch is on.
• Check that the power cord is properly connected.
• Check the building power supply.
If the cord if connected properly, and the building circuit for the
detector is operating normally, contact Agilent.

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 Troubleshooting 6

Ozone Generation Problems

Before troubleshooting the ozone generator, first verify that the
other components of the system operate normally. For example,
check for leaks in the detector external connections, check for
leaks in the inlet and inlet column fitting, check that the
vacuum pump operates normally, check that the inlet and ALS
are operating normally, and so on.
Troubleshoot ozone generation as follows:
1 On the display, note the detector output signal.
2 Leave the vacuum pump on and ozone supply gas flowing.
3 Turn off the ozone generator.
4 Observe the detector output signal.
5 Turn on the ozone generator and check the detector output
signal again.
A properly operating detector will typically display a difference
in background signal between ozone supply gas voltage on and
off. If no change is observed, contact Agilent service.

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6 Troubleshooting

Coking
Contamination from some sample matrices can reduce
sensitivity. For example, crude oils containing volatile metal
complexes may contaminate the ceramic tubes. In addition,
incomplete combustion of certain hydrocarbon-containing
compounds leaves behind coke deposits on the ceramic tubes.
Coke deposits may be removed from the burner by reducing the
hydrogen flow rate.

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 Troubleshooting 6

Hydrogen Poisoning
Hydrogen poisoning of the SCD ceramic tubes can occur when
the relative oxidizer flow is very much lower than the hydrogen
flow. Whether this state occurs due to inappropriate method
setpoints or due to a problem with the oxidizer flow, this
condition results in extremely reduced or no response. If you
suspect hydrogen poisoning:
• Check for and resolve any flow shutdown.
• Check for restrictions in the oxidizer supply line to the
burner assembly.
• Load the checkout method or other method that uses more
balanced relative flow rates.
If the response does not recover, replace the inner ceramic tube.
If response still does not recover, replace the outer ceramic
tube. The ceramic tubes cannot be reconditioned.

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6 Troubleshooting

Contaminated Gases
Agilent recommends the use of clean gases that meet the
requirements in the Site Preparation Guide. In addition,
Agilent highly recommends the use of high quality traps to
eliminate as much possible contamination as possible. The use
of clean gases is essential for optimal performance. Otherwise,
sulfur and other contaminants from gases may accumulate in
the column and bleed out over time, desensitizing the ceramic
tubes and causing elevated baselines.
Moisture in the ozone generator supply line can lead to the
formation of acids that can damage or destroy the ozone
generator and other detector components. Agilent highly
recommends the use of a high-quality moisture trap, such as the
Gas Clean Filter System with a moisture trap, for the ozone
supply gas. See “Consumables and Replacement Parts” on
page 56.

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Agilent 8355 S SCD and 8255 S NCD
User Manual

7
Performance Verification
About Chromatographic Checkout 96
Prepare for Chromatographic Checkout 97
Check SCD Performance 99
Check NCD Performance 105






This chapter describes how to verify that the detector is

operating normally.

Agilent Technologies 95
7 Performance Verification

About Chromatographic Checkout

The tests described in this section provide basic confirmation
that the detector can perform comparably to factory condition.
However, as detectors and the other parts of the GC age,
detector performance can change. The results presented here
represent typical outputs for typical operating conditions and
are not specifications.
The tests assume the following:
• Use of an automatic liquid sampler. If not available, use a
suitable manual syringe instead of the syringe listed.
• Use of a 10-μL syringe in most cases. However, a 5-μL syringe
is an acceptable substitute.
• Use of the septa and other hardware (liners, adapters, and so
forth) described. If you substitute other hardware,
performance can vary.

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 Performance Verification 7

Prepare for Chromatographic Checkout

Because of the differences in chromatographic performance
associated with different consumables, Agilent strongly
recommends using the parts listed here for all checkout tests.
Agilent also recommends installing new consumable parts
whenever the quality of the installed ones is not known. For
example, installing a new liner and septum ensures that they
will not contribute any contamination to the results.

The parts listed here apply to Agilent GCs. For other GC types, match part
NOTE
properties as appropriate.

1 Check the indicators/dates on the gas supply traps. Replace

expended traps.
2 Install new consumable parts for the inlet and prepare the
correct injector syringe (and needle, as needed).

Table 9 Recommended parts for checkout by inlet type

Recommended part for checkout Part number

Split splitless inlet
Syringe, 10-µL 5181-1267
Liner O-ring 5188-5365
Septum, bleed and temperature optimized (BTO), 5183-4757
non-stick
Liner, Ultra Inert, splitless, single taper, glass wool 5190-2293
Gold plated inlet seal, with washer 5188-5367
Multimode inlet
Syringe, 10-µL 5181-1267
Liner O-ring 5188-5365
Septum 5183-4757
Liner, Ultra Inert, splitless, single taper, glass wool 5190-2293
Cool On-column inlet
Septum 5183-4758
Septum nut 19245-80521
Syringe, 5-µL on-column 5182-0836

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7 Performance Verification

Table 9 Recommended parts for checkout by inlet type (continued)

Recommended part for checkout Part number

0.32-mm needle for 5-µL syringe 5182-0831
7693A ALS: Needle support insert, COC G4513-40529
7683B ALS: Needle support assembly for G2913-60977
0.25/0.32 mm injections
Insert, fused silica, 0.32-mm id 19245-20525

Prepare sample vials

Performance verification requires a 1 uL injection.

WA RNING When handling checkout standards, always follow the handling

precautions recommended with its packaging.

1 Open the sample box.

2 Snap the top off of one checkout sample ampoule.
3 Transfer the contents to a 2-mL ALS sample vial and cap the
vial.

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 Performance Verification 7

Check SCD Performance

1 Gather the following:
• Evaluation column, DB-1 30 m × 0.32 mm × 1.0 μm (part
number 123-1033)
• SCD performance evaluation (checkout) sample
(5190-7003): 0.7 ± 0.002 mg/L diethyl disulfide and
1.0 ± 0.003 mg/L tert-butyldisulfide in isooctane.
• Chromatographic-grade isooctane
• 4-mL solvent and waste bottles or equivalent for
autoinjector
• 2-mL sample vials or equivalent for sample
• Inlet and injector hardware (See “Prepare for
Chromatographic Checkout” on page 97.)
2 Verify the following:
• Chromatographic-grade gases plumbed and configured:
helium as carrier gas, air as oxidizer, and oxygen as ozone
supply gas.
• Ozone supply gas moisture trap and other traps are in
date.
• Empty waste vials loaded in sample turret.
• 4-mL solvent vial with diffusion cap filled with isooctane
and inserted in Solvent A injector position.
• 4-mL solvent vial with diffusion cap filled with isooctane
and inserted in Solvent B injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and
so forth) as needed for the checkout. See “Prepare for
Chromatographic Checkout” on page 97.
4 Install the evaluation column. (See the procedure for in the
GC Maintaining Your GC manual.)
• Bake out the evaluation column for at least 30 minutes at
180 °C. (See the procedure for in the GC Maintaining
Your GC manual.)
• Configure the column.
5 Check the detector baseline output. The output should be
below 150 pA and relatively stable, assuming a
well-stabilized system with the column oven at 50 °C.
However, a new burner (or a burner with a new ceramic
tube) can have a very high baseline after first ignition. In this
case, the baseline should gradually decrease, depending on

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7 Performance Verification

burner cleanliness. Noise will also greatly decrease over time.

For a well-stabilized system, noise measured by Agilent
OpenLAB CDS should be approximately 5 display units or
less.
Checkout can continue before the baseline becomes
completely stable.
6 Set the analog range to 9, if using an AIB. If using an Agilent
35900E A to D set to 10, or set to 12 if testing for linearity.
This starting point may require adjustment.
7 Create or load a method with the parameter values listed in
Table 10.

Table 10 SCD Checkout conditions

Column and sample

Type DB-1, 30 m × 0.32 mm × 1 µm
(123-1033)
Sample SCD checkout 5190-7003
Column flow 2 mL/min helium
Column mode Constant flow
Split/splitless inlet
Temperature 250 °C
Mode Splitless
Purge flow 40 mL/min
Purge time 0.7 min
Septum purge 3 mL/min
Gas saver Off
Multimode inlet
Mode Splitless
Inlet temperature 250 °C
Purge time 0.7 min
Purge flow 80 mL/min
Septum purge 3 mL/min
Gas saver Off
Cool on-column inlet
Temperature Oven Track

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 Performance Verification 7

Table 10 SCD Checkout conditions (continued)

Septum purge 15 mL/min

Detector
Base temperature 280°C
Burner temperature 800 °C
Upper H2 flow 38 mL/min
Lower H2 flow 8 mL/min
Oxidizer flow 50 mL/min, Air
O3 Generator flow On
O3 Generator power On
Vacuum pump On
FID-SCD Tandem settings
FID temp 350 °C
FID hydrogen flow 35 mL/min
FID air flow 300 mL/min
FID N2 makeup flow 20 mL/min
SCD oxidizer flow 5 mL/min, Air
SCD upper H2 flow 40 mL/min
Lower H2 flow Not applicable for FID-SCD
Oven
Initial temp 50 °C
Initial time 3.0 min
Rate 1 25 °C/min
Ramp 1 temp 160 °C
Ramp 1 hold time 2 min
Post run temp 50 °C
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Sample wash volume 8 µL (maximum)
Injection volume 1 µL
Syringe size 10 µL
Solvent A pre washes 0

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7 Performance Verification

Table 10 SCD Checkout conditions (continued)

Solvent A post washes 3

Solvent A wash volume 8 µL (maximum)
Solvent B pre washes 0
Solvent B post washes 3
Solvent B wash volume 8 µL (maximum)
Injection mode (7693A) Normal
Airgap Volume (7693A) 0
Viscosity delay 0
Solvent Wash Draw Speed (7693A) 150
Solvent Wash Dispense Speed 1500
(7693A)
Sample Wash Draw Speed (7693A) 150
Sample Wash Dispense Speed 1500
(7693A)
Inject Dispense Speed (7693A) 3000
Plunger speed (7683) Fast, for all inlets except COC.
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 µL
Data system
Data rate 5 Hz (Front detector, SCD)

8 If using a data system, prepare the data system to perform

one run using the loaded checkout method. Make sure that
the data system will output a chromatogram. If not using a
data system, create a one sample sequence using the GC
keypad.
9 Start the run. If performing an injection using an
autosampler, start the run using the data system or press
[Start] on the GC. If performing a manual injection (with or
without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 μL of the checkout
sample and press [Start] on the GC.

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 Performance Verification 7

The following chromatogram shows typical results for a new

detector with new consumable parts installed. Note that the
response for a tandem FID-SCD installation will be
approximately 1/10 of the response shown in this example
due to the reduced amount of sample that reaches the SCD.

SCD1 A, Front Signal (C:\CHEM32\2\DATA\XCD-DATA-FEB2015\SCD\EXAMPLE.D)

7 .8 0 6

tert-butyldisulÀde
6 .1 0 1
diethyl disulÀde
2500

2000

1500

1000

500

2.5 5 7.5 10 min

For a new installation, calculate the MDL of sulfur for the

detector. Calculate MDL as:

2 x noise
MDL =
sensitivity

where
noise is the ASTM noise calculated by the Agilent data system
Sensitivity is calculated as:

peak area
Sensitivity =
amount

Based on the 1 μL injection of the checkout standard, typical

results of the MDL calculations are shown in the table below.

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7 Performance Verification

Compound Amount injected Sulfur S amount Typical ASTM Typical Typical MDL
(mg/L) content injected noise Sensitivity (pg S/µL)
(pg/µL) (Area/pg*s)
Diethyl disulfide 0.700 52.50 % 367.500 2.453 9.504 0.469
tert-Butyldisulfide 1.000 36.00 % 360.000 2.453 10.993 0.446

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 Performance Verification 7

Check NCD Performance

1 Gather the following:
• Evaluation column, HP-5 30 m × 0.32 mm × 0.25 μm (part
number 19091J-413)
• NCD performance evaluation (checkout) sample
(5190-7002): 3-methylindole 10.0 ± 0.1 mg/L,
9-methylcarbazole 14.1 ± 0.1 mg/L, and nitrobenzene
9.51 ± 0.05 mg/L in isooctane.
• Chromatographic-grade isooctane
• 4-mL solvent and waste bottles or equivalent for
autoinjector
• 2-mL sample vials or equivalent for sample
• Inlet and injector hardware (See “Prepare for
Chromatographic Checkout” on page 97.)
2 Verify the following:
• Chromatographic-grade gases plumbed and configured:
helium as carrier gas, oxygen as oxidizer and ozone supply
gas.
• Ozone supply gas moisture trap and other traps are in
date.
• Empty waste vials loaded in sample turret.
• 4-mL solvent vial with diffusion cap filled with isooctane
and inserted in Solvent A injector position.
• 4-mL solvent vial with diffusion cap filled with isooctane
and inserted in Solvent B injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and
so forth) as needed for the checkout. See “Prepare for
Chromatographic Checkout” on page 97.
4 Install the evaluation column. (See the procedure for in the
GC Maintaining Your GC manual.)
• Bake out the evaluation column for at least 30 minutes at
270 °C. (See the procedure for in the GC Maintaining
Your GC manual.)
• Configure the column.
5 Check the detector baseline output. The output should be
below 150 pA and relatively stable, assuming a
well-stabilized system with the column oven at 50 °C. (A
negative baseline can be acceptable.).

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7 Performance Verification

However, a new burner (or a burner with a new quartz tube)

can have a very high baseline after first ignition. In this case,
the baseline should gradually decrease, depending on burner
cleanliness. Noise will also greatly decrease over time. For a
well-stabilized system, noise measured by Agilent OpenLAB
CDS should be approximately 4 display units or less.
Checkout can continue before the baseline becomes
completely stable.
6 Set the analog range to 9, if using an AIB. If using an Agilent
35900E A to D set to 10, or set to 12 if testing for linearity.
This starting point may require adjustment.
7 Create or load a method with the parameter values listed in
Table 11.

Table 11 NCD Checkout conditions

Column and sample

Type HP-5, 30 m × 0.32 mm × 0.25 µm
(19091J-413)
Sample NCD checkout 5190-7002
Column flow 2.2 mL/min
Column mode Constant flow
Split/splitless inlet
Temperature 250 °C
Mode Splitless
Purge flow 80 mL/min
Purge time 0.8 min
Septum purge 3 mL/min
Gas saver Off
Multimode inlet
Mode Splitless
Inlet temperature 250 °C
Initial time 0 min
Purge time 0.8 min
Purge flow 80 mL/min
Septum purge 3 mL/min
Gas saver Off

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 Performance Verification 7

Table 11 NCD Checkout conditions (continued)

Cool on-column inlet

Temperature Oven Track
Septum purge 15 mL/min
Detector
Base temperature 280°C
Burner temperature 900 °C
Chiller temperature On
H2 flow 3 mL/min
Oxidizer flow 8 mL/min, Oxygen
O3 Generator flow On
O3 Generator power On
Vacuum pump On
Oven
Initial temp 50 °C
Initial time 3.0 min
Rate 1 25 °C/min
Ramp 1 temp 250 °C
Ramp 1 hold time 2 min
Post run temp 50 °C
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Sample wash volume 8 µL (maximum)
Injection volume 1 µL
Syringe size 10 µL
Solvent A pre washes 0
Solvent A post washes 3
Solvent A wash volume 8 µL (maximum)
Solvent B pre washes 0
Solvent B post washes 3
Solvent B wash volume 8 µL (maximum)
Injection mode (7693A) Normal

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7 Performance Verification

Table 11 NCD Checkout conditions (continued)

Airgap Volume (7693A) 0

Viscosity delay 0
Solvent Wash Draw Speed (7693A) 150
Solvent Wash Dispense Speed 1500
(7693A)
Sample Wash Draw Speed (7693A) 150
Sample Wash Dispense Speed 1500
(7693A)
Inject Dispense Speed (7693A) 3000
Plunger speed (7683) Fast, for all inlets except COC.
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 µL
Data system
Data rate 5 Hz (Front detector, NCD)

8 If using a data system, prepare the data system to perform

one run using the loaded checkout method. Make sure that
the data system will output a chromatogram. If not using a
data system, create a one sample sequence using the GC
keypad.
9 Start the run. If performing an injection using an
autosampler, start the run using the data system or press
[Start] on the GC.If performing a manual injection (with or
without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 μL of the checkout
sample and press [Start] on the GC.

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 Performance Verification 7

The following chromatogram shows typical results for a new

detector with new consumable parts installed.

NCD1 A, Front Signal (C:\CHEM32\2\DATA\XCD-DATA-FEB2015\NCD\EXAMPLE.D)

9-methylcarbazole
nitrobenzene

3-methylindole
4000

5.859

9.947
7.800
3000

2000

1000

0 2 4 6 8 10 min

For a new installation, calculate the MDL of nitrogen for the

detector. Calculate MDL as:

2 x noise
MDL =
sensitivity

where
noise is the ASTM noise calculated by the Agilent data system
Sensitivity is calculated as:

peak area
Sensitivity =
amount

Based on the 1 μL injection of the checkout standard, typical

results of the MDL calculations are shown in the table below.

8355 S SCD and 8255 S NCD User Manual 109

 Agilent Technologies

Compound Amount Nitrogen N amount Typical ASTM Typical Typical MDL

injected content injected noise Sensitivity (pg N/µL)
(mg/L) (pg/µL) (Area/pg*s)
Nitrobenzene 9.510 11.37 % 1081.29 1.080 2.813 0.7679
3-Methylindole 10.000 10.67 % 1067.00 1.080 2.668 0.810
9-Methylcarbazole 14.100 7.72 % 1088.52 1.080 2.795 0.773

Agilent Technologies, Inc.

Printed in USA
March 2017