Agilent Technologies 5500t User manual

Agilent 5500 Series
FTIR
Operation Manual

2 Agilent 5500 Series FTIR Operation Manual
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2013
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Manual Part Number
0020-401
Edition
Fifth edition, September 2013
Printed in Malaysia
Agilent Technologies, Inc.
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Contents
Agilent 5500 Series FTIR Operation Manual 3
Contents
1. Introduction 5
2. Getting Started 9
Unpacking 9
Agilent 5500t FTIR packing list 10
Agilent 5500a FTIR packing list 10
Connecting power 11
Power cord selection 13
Connecting the computer 14
Turning on the instrument 15
Power switch LED 15
Starting the software 16
Logging on to MicroLab PC for the first time 16
Performance verification 17
Diagnostic values 18
Performance validation 20
3. Analyzing Samples 23
Lube samples with the Agilent 5500t FTIR 23
Cleaning the TumblIR accessory 25
Collecting a background spectrum 26
Measuring a sample 26
Agilent 5500t FTIR with a TumblIR 28
Cleaning the accessory 29
Collecting a background spectrum 30

Contents
4 Agilent 5500 Series FTIR Operation Manual
Measuring a liquid sample 31
Agilent 5500a FTIR with an ATR 33
Cleaning the accessory 36
Collecting a background spectrum 36
Collecting a sample spectrum 37
Agilent 5500 DialPath FTIR 39
Cleaning the DialPath accessory 41
Collecting a background spectrum 43
Measuring a liquid sample 43
4. Spare Parts 47
5. Specifications 49
Environmental conditions 50
Electromagnetic compatibility 50
ICES/NMB-001 51

Introduction
Agilent 5500 Series FTIR Operation Manual 5
1. Introduction
The Agilent 5500 Series FTIR instruments are small sized, mid-
infrared region spectrometer platforms specifically designed to
provide the capabilities of much larger, traditional FTIR
spectrometers, but without the complexity, maintenance
requirements or cost. The instrument dimensions are only 20.3 x 20.3
x 11.4 centimeters (8.0 x 8.0 x 4.5 in) high and it is very lightweight
(3.6 kg; 8 lb). Although the hardware platforms are in many ways the
same, the Agilent 5500t FTIR system is designed specifically for
onsite oil analysis, and the Agilent 5500a FTIR system is designed for
sample analysis in challenging, multi-user environments. Both
platforms provide versatility for use in a traditional analytical
chemistry laboratory, a temporary field laboratory or even in the
field. However, it is primarily intended for indoor use and is not
designed for water-resistance or other extreme outdoor conditions.
WARNING
Fire Hazard
5500 Series FTIR systems are NOT intrinsically safe. Use the system only in
atmospheres that have been tested for flammable materials. If the equipment
is used in a manner not specified in this manual, the protection provided by
the equipment may be impaired.

Introduction
6 Agilent 5500 Series FTIR Operation Manual
The 5500 Series FTIR systems use technology known as Fourier
transform infrared (FTIR) spectroscopy, which is the current state-
of-the-art technique for molecular compound identification and
quantification. FTIR uses an infrared (IR) light source to pass
through the sample and onto a detector, which precisely measures
the amount of light absorbed by the sample. This absorbance creates
a unique spectral fingerprint that is used to identify the molecular
structure of the sample and determine the exact quantity of a
particular compound in a mixture.
The heart of the Agilent FTIR spectrometer system is a patented,
rugged Michelson interferometer, field-proven for onsite and mobile
use. This proprietary design is the key to successfully making FTIR
technology compact, lightweight, rugged and field-portable.
The 5500 Series FTIR instruments are controlled using an external
computer running a Microsoft® Windows® XP (32- or 64-bit) or
Windows 7 (32- or 64-bit) operating system. The computer must have
at least a Pentium® IV 3 GHz processor with 1 GB of memory and at
least 40 GB hard disk capacity. The laptop computer is offered as an
option, which provides the flexibility of supplying it yourself or
purchasing from Agilent.
The 5500 FTIR system is available in a number of different sampling
configurations to accommodate the analysis of a range of liquids,
powders, pastes and gels. The optimal use of the various
configurations of the 5500 FTIR system are:
Agilent 5500t FTIR TumblIR System: For the rapid chemical
analysis of liquids under ambient conditions.
Agilent 5500a FTIR ATR System: For the chemical analysis of
liquids, powders, pastes and gels. The attenuated total
reflectance (ATR) system is available in single reflection (most
common), three reflection and nine reflection versions. The nine
reflection version has an optional flowcell configuration.
The Agilent 5500 DialPath FTIR is for the rapid chemical analysis of
liquids under ambient conditions that require multiple pathlengths.

Introduction
Agilent 5500 Series FTIR Operation Manual 7
The 5500t FTIR system is a TumblIR liquid cell accessory-based
instrument specifically designed for onsite oil analysis. This system is
an ideal tool for oil analysis of diesel generators, wind farms, off-
shore applications or marine applications.
Both systems are equipped with a software user interface that is
intuitive, simple to use and requires no specialized technical training.
With the touch of a button, the system provides valuable information
about the identity and amount of chemical substances present in a
material.

Introduction
8 Agilent 5500 Series FTIR Operation Manual
This page is intentionally left blank.

Getting Started
Agilent 5500 Series FTIR Operation Manual 9
2. Getting Started
Unpacking 9
Connecting power 11
Connecting the computer 14
Turning on the instrument 15
Starting the software 16
Performance verification 17
Unpacking
To unpack your spectrometer system:
1After receiving the Agilent 5500 Series FTIR delivery, do not
immediately open the shipping container. Instead, place the
shipment in a room-temperature environment and allow several
hours for the contents of the container to reach the room
ambient temperature. This is to avoid unnecessary condensation
on the components prior to the initial setup and installation
process.
2The shipping enclosure should contain the items listed below.
Inspect the enclosure closely to make sure all items have been
removed from the shipment packaging. Also ensure that all the
items in the packing list below have arrived undamaged and are
in good working condition. Contact Agilent immediately if any
items are found to be missing in shipment or damaged.
NOTE Keep all original packing material for storing, shipping and transporting the
system in the future.

Getting Started
10 Agilent 5500 Series FTIR Operation Manual
3Remove the 5500 Series FTIR system from its shipping case and
place it on a flat, stable surface. The instrument must be kept
away from hot surfaces and any sources of electromagnetic
interference.
Agilent 5500t FTIR packing list
One Agilent 5500t FTIR mid-IR spectrometer system, including
TumblIR sampling accessory
One Agilent 5500 Series FTIR Operation Manual
One power cord
One USB cable
One installation disk
One shipping container
Options
Although the spectrometer system comes standard as shown above,
there are a number of options available, including:
Laptop computer
Surfactant kit
Extra cords
Agilent 5500a FTIR packing list
One Agilent 5500a FTIR mid-IR spectrometer system, including
appropriate sampling accessory
One Agilent 5500 Series FTIR Operation Manual
One power cord
One USB cable
One installation disk
One shipping container

Getting Started
Agilent 5500 Series FTIR Operation Manual 11
Options
Although the spectrometer system comes standard as shown above,
there are a number of options available, including:
Laptop computer
Single-bounce ATR (includes sample press)
Multi-bounce or 9 bounce ATR
Extra cords
To convert your 5500a FTIR system to a different accessory, contact
Agilent.
Connecting power
To connect power to the spectrometer system:
1Insert the provided power cord into the power connector located
on the lower left side at the rear of the 5500 Series FTIR system
(see Figure 1).
Figure 1. Attaching the power cord
2Thread the blue cap onto the power connector by rotating it
clockwise until finger-tight. To avoid damage to the plastic
connector, be careful not to over-tighten.

Getting Started
12 Agilent 5500 Series FTIR Operation Manual
3The appropriate power supply cabling will be provided with the
system. Connect the opposite end of the power cable to the AC
power outlet.
CAUTION To prevent any power startup damage or problems, connect the power cord to
the spectrometer system first and then to the power outlet.
CAUTION To avoid damage to the system due to power surges or a faulty power source,
always use a UL approved power surge protection strip between the power
outlet source and the system power cord.
CAUTION All cords must be kept away from high traffic areas. The system could sustain
damage to the apparatus or adapters if excessive strain to the power cord
connections occurs.

Getting Started
Agilent 5500 Series FTIR Operation Manual 13
Power cord selection
The following power cords can be used:
Figure 2. Suitable power cords

Getting Started
14 Agilent 5500 Series FTIR Operation Manual
Connecting the computer
To connect the instrument to the computer:
1Insert the provided USB cable into the USB connector located on
the upper left side at the rear of the 5500 Series FTIR system (see
Figure 3).
Figure 3. Attaching the USB cable
2Thread the blue cap onto the USB connector by rotating it
clockwise until finger-tight. To avoid damage to the plastic
connector, be careful not to over-tighten.
3Connect the opposite end of the USB cable to the computer that
will run MicroLab PC software.
NOTE The 5500t FTIR must be directly connected to the computer USB slot and NOT
through a USB hub or adapter.

Getting Started
Agilent 5500 Series FTIR Operation Manual 15
Turning on the instrument
Press the green power button located on the front of the 5500 Series
FTIR system and hold for two seconds. The LED light will illuminate
green when the system is activated.
Press the power button to turn off the 5500 Series FTIR system — the
light will turn red. During a firmware update, the light will turn red
and blink.
CAUTION The power button is a momentary switch to avoid accidental power off. In order
to turn the system on or off, hold the button down for two (2) seconds.
Power switch LED
The power button contains a two-colored LED. The color displayed
on the LED can indicate the state of the system. Table 1 lists the
colors of the LED and the status of the instrument.
Table 1. Power switch LED status
Status LED color Action (% duty cycle)
System OFF No LED illumination N/A
System OFF Red 100%
System startup Red/green Green 0.5 s on / Red 0.5 s on
System ON Green 100%
Low battery Green 50% (0.5 s on / 0.5 s off)
Critically low battery Red 50% (0.5 s on / 0.5 s off)
Dead battery No LED illumination N/A
Firmware update Red/green Green blinks rapidly twice then red blinks
rapidly twice

Getting Started
16 Agilent 5500 Series FTIR Operation Manual
Starting the software
To start the software:
1Ensure that the system is active, then double-click the MicroLab
PC icon.
2The system must have a warmup period of 5 minutes, before
analysis may begin.
Logging on to MicroLab PC for the first time
The 5500 Series FTIR systems are supplied with the Agilent MicroLab
PC software, which has already been installed on your external
laptop computer.
In addition, the system is provided with a shortcut to the MicroLab
PC software in the Start menu.
Upon initial power up of the spectrometer system, the MicroLab PC
software application splash screen briefly appears, showing the
version, copyright and trademark information. The software will
launch and display a logon screen.
When the logon screen appears, the user name will be ‘Admin’ –
when logging onto the system for the first time, the software
automatically initiates in an Administrator mode. The default
password for initial logon to MicroLab PC software is ‘admin’.
NOTE The user name and password are case-sensitive.
For detailed instructions on initial software logon and user
management, refer to the MicroLab Software Operation Manual.
For additional instructions on adding a user to the system and other
initial software setup procedures, plus editing methods and
reviewing data using MicroLab PC software, refer to the MicroLab
Software Operation Manual.

Getting Started
Agilent 5500 Series FTIR Operation Manual 17
Performance verification
The 5500 Series FTIR spectrometer systems have been thoroughly
tested at the factory, so no alignment steps are required. However, it
is recommended to run the performance test initially to ensure the
instrument is running properly. To run and interpret the
performance test, refer to the MicroLab Software Operation Manual.
The performance test measures the energy level of the instrument
(based on the interferogram voltage or height). A successful test will
be indicated by a green circle at the top of the software screen. You
are now ready to analyze a sample. A yellow or red circle indicates
the instrument is operating outside of the factory defined
parameters. These parameters are listed on the Advanced Features
software page.
NOTE If the circle at the top of the software screen is yellow or red, contact Agilent
technical support for assistance.
Like any measurement device, it is important to verify that the 5500
Series FTIR instrument is performing properly before using the
system to make critical measurements. The instrument provides both
diagnostic values and performance validation tests to demonstrate
the system’s performance. The diagnostic values provide an easy to
understand, quick assessment of the instrument’s function. If the
instrument is not functioning properly, one of the diagnostic values
will be out of specification. Typically, the instrument will not allow
data collection if the diagnostic values are out of specification.
Performance validation tests are longer, more involved tests that
measure how well the instrument is working. The tests listed under
‘Performance validation’ check the instrument’s sensitivity
(performance), stability and frequency precision (laser calibration).

Getting Started
18 Agilent 5500 Series FTIR Operation Manual
Each industry has different requirements for instrument verification.
In general, the diagnostic values should be checked on a daily or
weekly basis. The instrument will not collect data if the diagnostic
values are grossly out of specification, but it is good practice to verify
that the instrument is working properly. Performance validation
should be run on a quarterly or bi-annual basis. Highly-regulated
industries may require the performance validation to be run
monthly, depending on the use of the instrument. The performance
validation verifies the key aspects to the instrument’s ability to
measure good data. If the performance validation tests are within
specification, the instrument should provide data that works well
with methods developed for the 5500 Series FTIR spectrometer. As
with any instrument; however, results can always be verified by
running a known sample with the sample specific method.
Diagnostic values
The following values can also be viewed from the Diagnostics page in
the MicroLab PC software. These values can be used to determine if
the instrument is working properly. They can be used on a daily basis
to determine that the instrument is operating as intended. In each
case, the Optimal value indicates that the system is running at its
intended performance level. The Marginal value indicates that the
instrument is still functioning, but at a lower performance level. The
Critical value indicates that the system is not working correctly.
Contact Agilent technical support for assistance if there is a problem
with your instrument.

Getting Started
Agilent 5500 Series FTIR Operation Manual 19
Table 2. Diagnostic values
Value Optimal (green) Marginal (yellow) Critical (red) Comment
Energy
(centerburst)
26,000
–
21,000 >30,000or
< 15,000
> 31,000 or
< 10,000
Indicates the overall
alignment and proper gain
adjustment for the system.
Battery life AC or
>30 min
30
–
5 min <5 min
Source 1.9 A >2.2 or
<1.6
>2.5 or
<1.0
Indicates a problem with
the source control voltage
or that the source has
burnt out. Both voltage and
amperage are displayed;
however, amperage
provides a sufficient
diagnostic.
Laser signal 15,000
–
3,000 >15,000 or
<3,000
>17,000 or
< 2,000
Can verify gross alignment
errors even if the
reflectance cap is not in
place.
Detector
temperature
35
–
44 <35
or >44
<30
or >48
Indicates a problem with
the cooling circuitry or an
ambient temperature over
the specified range.
CPU
temperature
10
–
75 >75 >80 Indicates the ambient
temperature over the
specified range.

Getting Started
20 Agilent 5500 Series FTIR Operation Manual
Performance validation
The MicroLab PC software has three tests appropriate for
performance validation of the instrument. All of these tests can be
accessed from the Advanced Features, System Check page of the
MicroLab PC software. The 5500 Series FTIR system should be
warmed up for at least 30 minutes before conducting any of these
tests. These tests can be run on a quarterly, bi-annual or annual basis
to determine that the instrument is performing within its
specification.
Performance (signal-to-noise) test
This test measures the signal-to-noise level at two regions of the IR
spectrum: 2500 cm-1 and 1000 cm-1. The signal-to-noise is defined as
the reciprocal of the root mean squared (RMS) noise in the defined
region for a blank sample measured with a blank background. Both
the background and sample are measured at 4 cm-1 resolution with a
one minute collection time. This test takes 2 minutes per test. The
user can specify a number of tests to be conducted. For 45 degree
external reflectance and grazing angle reflectance measurements, the
appropriate reflective reference cap should be in place for the entire
test. No reference cap is needed when using the ATR sample
interface. At least 10 tests should be collected in order to obtain an
accurate picture of the performance.
Stability test
This test measures the short-term stability at two regions of the
spectrum: 3000 cm-1 and 1000 cm-1. Stability is a measurement of the
baseline differences observed over the selected time period. The test
measures a background at the beginning, then one sample every
minute for the duration of the test as specified in the ‘Number of
minutes’ field in the software. The test results are expressed as
%Transmittance (difference versus 100%) of maximum deviation
during the stability test.