Agilent Technologies 4500 Series User manual

Agilent 4500 Series
FTIR
Operation Manual

2 Agilent 4500 Series FTIR Operation Manual
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Manual Part Number
0021-401
Edition
Tenth edition, October 2017
Printed in Malaysia
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Contents
Agilent 4500 Series FTIR Operation Manual 3
Contents
1. Introduction 5
2. Getting Started 7
Unpacking 7
Agilent 4500t FTIR packing list 8
Agilent 4500a FTIR packing list 8
Agilent 4500 DialPath FTIR packing list 9
Connecting power 10
Power cord selection 12
Turning on the instrument 13
Power switch LED status 13
Starting the software 14
Performance verification 14
Diagnostic values 15
Performance validation 17
3. Analyzing Samples 19
Lube samples with the Agilent 4500t FTIR 19
Cleaning the TumblIR accessory 21
Collecting a background spectrum 22
Measuring a sample 22
Agilent 4500t FTIR with a TumblIR 24
Cleaning the accessory 25
Collecting a background spectrum 26
Measuring a liquid sample 27

Contents
4 Agilent 4500 Series FTIR Operation Manual
Agilent 4500a FTIR with an ATR 28
Cleaning the accessory 32
Collecting a background spectrum 32
Collecting a sample spectrum 33
Agilent 4500 DialPath FTIR 35
Cleaning the DialPath accessory 37
Collecting a background spectrum 39
Measuring a liquid sample 39
4. Spare Parts 43
5. Specifications and Safety Information 45
Specifications 45
Safety Information 46
Environmental conditions 46
Electromagnetic compatibility 46
EN55011/CISPR11 46
ICES/NMB-001 47

Introduction
Agilent 4500 Series FTIR Operation Manual 5
1. Introduction
The Agilent 4500 Series FTIR instruments are small sized, mid-
infrared region spectrometer platforms specifically designed for
portable, onsite chemical analysis outside the laboratory
environment. The systems are small (21.6 x 29.2 x 19.1 cm; 8.5 x 11.5
x 7.5 in), lightweight (6.8 kg; 15 lb) and packaged in a weather-
resistant enclosure suitable for outdoor use. They come standard
with internal battery power for operation of up to 4 hours or can be
operated with 110/220 volt AC power for extended use.
WARNING
Fire Hazard
4500 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.
The 4500 Series FTIR instruments 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.

Introduction
6 Agilent 4500 Series FTIR Operation Manual
The heart of the Agilent FTIR spectrometer system is a patented
Michelson interferometer design mounted on shock-dampening
mechanisms to protect the components from shock and vibration in
the field. This proprietary design is the key to successfully making
FTIR technology compact, lightweight, rugged and field-portable.
The 4500 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 4500 FTIR system are:
Agilent 4500t FTIR TumblIR System: For the rapid chemical
analysis of liquids under ambient conditions. The Agilent 4500t
FTIR is a TumblIR 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.
Agilent 4500a 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) or three reflection versions.
The Agilent 4500 DialPath FTIR is for the rapid chemical
analysis of liquids under ambient conditions that require
multiple pathlengths.
All 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.

Getting Started
Agilent 4500 Series FTIR Operation Manual 7
2. Getting Started
Unpacking 7
Connecting power 10
Turning on the instrument 13
Starting the software 14
Performance verification 14
Unpacking
To unpack your spectrometer system:
1After receiving the Agilent 4500 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.
3Remove the 4500 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.

Getting Started
8 Agilent 4500 Series FTIR Operation Manual
Locate the PC keyboard and mouse for ergonomically correct access.
Agilent 4500t FTIR packing list
One Agilent 4500t FTIR mid-IR spectrometer system, including
TumblIR sampling accessory
One Agilent 4500 Series FTIR Operation Manual
One power cord
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 4500a FTIR packing list
One Agilent 4500a FTIR mid-IR spectrometer system, including
appropriate sampling accessory
One Agilent 4500 Series FTIR Operation Manual
One power cord
One installation disk
One shipping container

Getting Started
Agilent 4500 Series FTIR Operation Manual 9
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 ATR
Extra cords
Agilent 4500 DialPath FTIR packing list
One Agilent 4500 DialPath FTIR mid-IR spectrometer system,
including DialPath accessory
One Agilent 4500 Series FTIR Operation Manual
One power cord
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
Extra cords

Getting Started
10 Agilent 4500 Series FTIR Operation Manual
Connecting power
To connect power to the spectrometer system:
1Before connecting the power cord to the power source, remove
the connector cap and then insert the power cord female
connector provided into the male power plug located on the left
side of the spectrometer system.
2Connect the other end of the power cord to the power source.
The appropriate power supply for your location will be provided
with the system. When the system is not in field use, keep it
plugged in to the local AC power to ensure a fully-charged battery
pack (see Figure 1).
Figure 1. Attaching the power cord
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.
Power button
USB
Power

Getting Started
Agilent 4500 Series FTIR Operation Manual 11
Once AC power is connected, the power button located next to the
power and USB connectors on the left side of the 4500 FTIR, will
appear a solid red color. This means the battery pack is being
charged, but the instrument is off.
NOTE The 4500t FTIR contains a Molicel lithium-ion rechargeable battery pack. Agilent
have fully charged the 4500t system prior to shipment, but the system should
also be plugged into a power outlet when not in use. The 4500t battery life under
continuous use is approximately 3.5 hours. It is recommended to allow the
battery pack to be re-charged at initial setup prior to turning on the power to the
instrument.
Molicel lithium-ion rechargeable battery pack specifications:
Capacity (nominal): 6600 mAh
Nominal voltage: 11.1 V
Energy: 73.2 Wh
Size: 149.5 x 89.3 x 20 mm
(5.8 x 3.5 x 0.8 in)
Weight: 480 g (1.1 lb)
Battery operating specifications:
Operating voltage: 12.6 to 9.0 V
Charge voltage: 12.6 V
Cutoff voltage: 7.5 V
Temperature range
Discharge: -20 to 60 °C (-4 to 140 °F)
Charge: 0 to 45 °C (32 to 113 °F)
Maximum discharge current: 3.5 A
(continuous)
Maximum charge current: 3.5 A

Getting Started
12 Agilent 4500 Series FTIR Operation Manual
Power cord selection
The following power plugs can be used:
Figure 2. Suitable power cords
When replacing the mains power cord, use only a mains power cord
with a rating equivalent to the one supplied with the instrument.

Getting Started
Agilent 4500 Series FTIR Operation Manual 13
Turning on the instrument
To turn on the instrument:
1Press the power button of the 4500 Series FTIR system and hold
for two (2) seconds. Initially the light will blink between red and
green while the firmware is being loaded. This process should
take less than 30 seconds. When the LED light illuminates solid
green, the instrument is now ready to use.
2The spectrometer must have a warmup period of 5 minutes
before reliable analysis may begin.
When finished using the instrument, press the green power button
again to turn off the system. The LED light will then turn red.
Power switch LED status
The power button contains a two-colored LED. The color displayed
on the LED can indicate the state of the system. The table below 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
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.

Getting Started
14 Agilent 4500 Series FTIR Operation Manual
Starting the software
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, refer to the MicroLab Software
Operation Manual.
Performance verification
The 4500 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.

Getting Started
Agilent 4500 Series FTIR Operation Manual 15
Like any measurement device, it is important to verify that the 4500
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).
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 4500 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 on 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
16 Agilent 4500 Series FTIR Operation Manual
Table 2. Diagnostic values
Value Optimal (green) Marginal (yellow) Critical (red) Comment
Energy
(centerburst)
26,000
–
21,000 >30,000 or
<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
Agilent 4500 Series FTIR Operation Manual 17
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 4500 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. 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.

Getting Started
18 Agilent 4500 Series FTIR Operation Manual
Laser Frequency Calibration test
The Laser Frequency Calibration test measures the frequency (X-
axis) accuracy. The test is conducted by measuring a spectrum of a
polystyrene film. Absorbance frequencies from this spectrum are
compared to frequencies set by NIST SRM 1921 polystyrene film. The
software allows administrative-level users to use the test results to
set the laser calibration. Laser calibrations should only be set after
consultation with an Agilent technical support engineer. For this test,
a background is measured first. After the background collection, a
spectrum of polystyrene film is measured as instructed by the
software. The polystyrene test sample must be pressed firmly against
the diamond sample interface during the sample collection.

Analyzing Samples
Agilent 4500 Series FTIR Operation Manual 19
3. Analyzing Samples
Lube samples with the Agilent 4500t FTIR 19
Agilent 4500t FTIR with a TumblIR 24
Agilent 4500a FTIR with an ATR 28
Agilent 4500 DialPath FTIR 35
Lubrication samples with the Agilent 4500t FTIR
The Agilent 4500t FTIR instrument is provided with a dedicated oil
and lubrication sampling interface called the TumblIR. The TumblIR
is a proprietary liquid transmission sampling accessory designed and
manufactured exclusively by Agilent to optimize the analysis of
lubrication samples. When comparing the TumblIR to traditional
liquid cells for general analytical laboratories, the TumblIR makes it
much easier to prepare, load, analyze and clean the sample.
The TumblIR operates in two modes: sample loading/cleaning, and
sample analysis.
In the sample loading and cleaning mode, the TumblIR is rotated so
the accessory window is facing up (see Figure 3). It is in this position
that the sample mounting area can be easily accessed for loading the
sample into place and for cleaning the sampling surfaces before the
next sample is analyzed.

Analyzing Samples
20 Agilent 4500 Series FTIR Operation Manual
Figure 3. TumblIR with accessory window facing up
In the sample analysis mode, the TumblIR is rotated such that the
accessory optical window is facing down towards the 4500t FTIR
sample mounting area. In this position, infrared (IR) energy passes
through the sample making measurement possible. Be sure to rotate
the TumblIR arm completely around until it reaches the detent and
snaps into position. This detent keeps the accessory stationary
during sample measurement (see Figure 4).
Figure 4. TumblIR with accessory window facing down
Bottom window (2 mm diameter yellow
surface)
Top window