Agilent Technologies 4200 FlexScan User manual

Agilent 4200 FlexScan
FTIR
Operation Manual

2 Agilent 4200 FlexScan FTIR Operation Manual
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Manual Part Number
0024-401
Edition
Third edition, May 2013
Printed in Malaysia
Agilent Technologies, Inc.
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Contents
Agilent 4200 FlexScan FTIR Operation Manual 3
Contents
1. Introduction 5
2. Getting Started 9
Unpacking 9
Packing list 10
Components 11
Installing the battery12
Power switch LED status 13
Starting the software 14
Charging the handheld PC 15
Logging on to MicroLab Mobile for the first time 15
Performance verification 16
Diagnostic values 17
Performance validation 19
3. Analyzing Samples 23
External reflectance, grazing angle and diffuse reflectance 23
Reflectance standards and gain settings 24
Steps 25
Collecting a background spectrum 25
Collecting a sample spectrum 26
Internal reflectance (ATR) 27
Steps 28
Cleaning the sample probe 28
Collecting a background spectrum 29

Contents
4 Agilent 4200 FlexScan FTIR Operation Manual
Collecting a sample spectrum 30
Using the solid sample ATR press 31
4. Maintenance 35
5. Spare Parts 37
6. Specifications 39
Technical 39
Environmental conditions 40
Handheld PC data station 40

Introduction
Agilent 4200 FlexScan FTIR Operation Manual 5
1. Introduction
The Agilent 4200 FlexScan FTIR instrument is a portable, handheld,
battery-operated analyzer designed to measure a variety of solid and
liquid samples in locations difficult or impossible to analyze in a
laboratory. It can be used for quantitative or qualitative analysis of
materials. The system is small, lightweight and packaged in a
weather-resistant enclosure suitable for outdoor use. It comes
standard with internal battery power for operation of up to 4 hours.
The 4200 FlexScan FTIR can be safely used in operating
temperatures ranging from 0 to 50 degrees Celsius (32 to 122 degrees
Fahrenheit) and in humidity environments as high as 95% for
extended periods of time.
WARNING
Fire Hazard
4200 FlexScan 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 4200 FlexScan FTIR Operation Manual
CAUTION Although the 4200 FlexScan FTIR system is designed to withstand significant
shock and vibration found in a field environment, use caution when handling and
avoid dropping the system when it is out of the shipping case. Dropping the
system may result in equipment failure.
The 4200 FlexScan FTIR uses 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. In addition to the capability to measure samples onsite
that in the past were typically measured in the lab, this system is a
non-destructive tool (NDT) that allows the analysis to be performed
without damaging the sample.
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 4200 FlexScan FTIR system can be configured for a number of
different sampling configurations to accommodate the analysis of a
range of liquids, solids, powders, pastes and gels. Information on the
optimal use of the different sampling configurations of the 4200
FlexScan system is listed in the following categories:

Introduction
Agilent 4200 FlexScan FTIR Operation Manual 7
Agilent 4200 FlexScan FTIR External Reflectance System: For
the chemical analysis of solid or hard surface samples, especially
thickness measurement of thin coatings and films on reflective
surfaces. Typical applications include thickness measurement,
analysis of anodization of metals, and measurement of surface
cleanliness. The External Reflectance System uses a 45 degree
specular reflectance probe or a grazing angle specular reflectance
probe. The 45 degree probe is optimal for analysis of thin films
greater than 1 micron in thickness. Specular reflectance is an
ideal method for the analysis of surface contamination.
Agilent 4200 FlexScan FTIR Grazing Angle System: The grazing
angle sample interface works in a similar manner to the external
reflectance sample interface; however, the angle of incidence is
82 degrees. The increased angle of incidence increases. The
grazing angle probe is optimal for analysis of ultra thin films less
than 1 micron in thickness. The grazing angle probe should be
used when very low level contamination needs to be analyzed
(nanometer thickness levels).
Agilent 4200 FlexScan FTIR Internal Reflectance System: For
the chemical analysis of liquids, powders, pastes and gels. The
Internal Reflectance System uses a diamond optical sampling
probe that incorporates the attenuated total reflectance (ATR)
technique. This method is optimal for the identification of a
variety of samples and has the advantage that no sample
preparation is required to obtain the proper IR absorbance
levels. The diamond ATR probe for the 4200 FlexScan FTIR is a
single reflection ATR. The single reflection ATR sampling
technique is ideal for identification of thick or highly-absorbing
samples where small IR pathlengths are required (typically
2 micron depth of penetration).

Introduction
8 Agilent 4200 FlexScan FTIR Operation Manual
The 4200 FlexScan FTIR is equipped with a handheld PC (Socket
PDA) as standard and can be interfaced to the optional laptop
computer for development of new methods and for detailed viewing
and manipulating the spectra. The 4200 FlexScan software user
interface is intuitive, simple to use and requires no specialized
technical training. The spectral display is represented with easy to
read status bars and report formats, which increase ease of use on
the smaller handheld PC display. 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 4200 FlexScan FTIR Operation Manual 9
2. Getting Started
Unpacking 9
Components 11
Installing the battery 12
Power switch LED status 13
Starting the software 14
Performance verification 16
Unpacking
To unpack your spectrometer system:
1After receiving the Agilent 4200 FlexScan FTIR delivery, do not
immediately open the shipping container. Instead, place the
shipping case 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.
Your 4200 FlexScan FTIR has been packed to ensure that it
arrives at your facility ready to go to work. Custom foam inserts
protect the instrument from damage during travel. Whenever
your instrument is shipped via common carrier, it needs to be re-
packed in the shipping case. Using this case, your 4200 FlexScan
can be removed and re-packed in the case in a matter of seconds,
while maintaining instrument security.

Getting Started
10 Agilent 4200 FlexScan FTIR Operation Manual
2The shipping enclosure should contain the standard items listed
below as well as any optional items ordered. 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 or damaged in shipment.
NOTE Keep all original packing material for storing, shipping and transporting the
system in the future.
3Remove the 4200 FlexScan FTIR system from its shipping case
and place it on its side on a flat, stable surface. The instrument
must be kept away from hot surfaces and any sources of
electromagnetic interference.
Packing list
Plastic shipping case
One Agilent 4200 FlexScan FTIR spectrometer system
One Agilent 4200 FlexScan FTIR mirrored reference cap
One Agilent 4200 FlexScan FTIR diffuse reference cap
One Agilent 4200 FlexScan FTIR polystyrene frequency check
standard
Two Agilent 4200 FlexScan FTIR Li-ion batteries
One Agilent 4200 FlexScan FTIR Operation Manual
One Agilent MicroLab Software Operation Manual
One Socket handheld PC system (PDA)
One Agilent 4200 FlexScan FTIR wrist strap
One shipping container

Getting Started
Agilent 4200 FlexScan FTIR Operation Manual 11
Cardboard box
One handheld PC USB cable with power connector
One battery charger
One power supply for battery charger
One AC line cord
One installation disk (needed as backup copy only)
One Agilent 4200 FlexScan FTIR USB cable
Components
The 4200 FlexScan FTIR is designed to measure samples in a
handheld configuration. Sample measurement can be started using
the handle-mounted trigger or the handheld PC touch screen.
Figure 1.Agilent 4200 FlexScan FTIR
USB connection
Power on/off button
Trigger
(RETURN)
Optical
housing
Sample interface
Reference cap
Battery door latch
Handheld
PC (PDA)
Battery
compartment
Electrical
housing
Belt clip

Getting Started
12 Agilent 4200 FlexScan FTIR Operation Manual
Installing the battery
The 4200 FlexScan FTIR comes with two lithium-ion batteries, which
are fully charged. Each battery gives approximately 4 hours of run
time. A battery charger is also included; refer to the battery charger
manual for information on its operation. There is an LCD display on
the front of the battery indicating the level of charge. Five (5) bars
indicate a full charge.
The 4200 FlexScan FTIR has a door on the front of the handle. The
door on the front gives access to the system battery. The door must
remain closed and locked while the system is in use. The 4200
FlexScan should arrive with one battery in the shipping case.
To install the battery:
1Release the battery door tab on the top of the electrical housing
(see Figure 1).
2Slide the battery into the compartment with the tab of the battery
facing downward and towards the front side of the 4200
FlexScan FTIR. The V-grove on the top of the battery interfaces
with the tab on the top of the battery compartment.
3Slide the battery towards the back of the compartment until you
feel the battery engage.
4Continue to slide another eighth of an inch until completely
engaged. If the battery is not fully engaged, the system will not
operate properly.
5Close the battery compartment door.
Depending on temperature and age of the battery, the system should
generally operate for a period of four hours on battery power.
To remove the battery from the compartment, open the door and pull
on the black plastic tab to slide the battery out of the 4200 FlexScan
FTIR housing.

Getting Started
Agilent 4200 FlexScan FTIR Operation Manual 13
WARNING
Electrical Shock Hazard
Avoid shock hazard. Never allow liquid to run into the 4200 FlexScan FTIR
battery compartment.
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.
NOTE The 4200 FlexScan FTIR contains a lithium-ion rechargeable battery pack. Agilent
has fully charged the 4200 FlexScan system prior to shipment. The 4200 FlexScan
battery life under continuous use is approximately 4 hours.

Getting Started
14 Agilent 4200 FlexScan FTIR Operation Manual
Starting the software
The 4200 FlexScan FTIR systems are supplied with the Agilent
MicroLab Mobile software, which has already been installed on your
handheld PC.
To start the software once the 4200 FlexScan FTIR has been
powered up:
1Turn on the handheld PC data station by depressing the power
button on the top right corner of the data station (see Figure 2).
Figure 2. Data station showing power button location
2The system is provided with a shortcut to the MicroLab Mobile
software in the Start menu. Upon initial power-up of the
handheld PC, look in the computer display window and tap
Start. Then tap the MicroLab Mobile icon. This will launch the
MicroLab Mobile software application.
NOTE
If the you see this message upon loading your software:
Instrument failed to initialize. Instrument returned error code: -2. The application
will exit; then power-cycle the instrument and restart the application.
the spectrometer is not connected to the computer. When using the handheld PC
with MicroLab Mobile, verify that the instrument displays a green light on the
power button and verify that the ‘Bluetooth’ communications of the handheld PC
are turned ‘On’. The instrument must be connected via Bluetooth for the
MicroLab Mobile software to launch.
Power button

Getting Started
Agilent 4200 FlexScan FTIR Operation Manual 15
Charging the handheld PC
To connect the handheld PC to an AC power source for charging
the battery:
1Connect the USB cable to the handheld PC.
2Connect the computer AC power cable to the ‘Y’ connector of the
USB cable.
3Connect the handheld PC power cable to the AC power source.
Alternatively, if purchased, place the PC in the optional handheld
charging cradle. For more information on the operation of the
handheld PC, see the supplied Socket User Manual.
Logging on to MicroLab Mobile for the first time
As mentioned above, the 4200 FlexScan FTIR systems are supplied
with the Agilent MicroLab Mobile software already installed on your
system. (A software disk for the Agilent MicroLab PC software is also
included. This allows use of the 4200 FlexScan with a desktop or
notebook computer.)
In addition, the handheld PC is provided with a shortcut to the
MicroLab Mobile software already installed in the Start menu.
To start the software:
1Tap Start then tap the MicroLab Mobile icon.
Upon initial launch of the system, the MicroLab Mobile software
automatically loads and a MicroLab application splash screen
appears briefly showing software version, copyright and trademark
information.
The software will launch and display a logon screen.
NOTE If the 4200 FlexScan FTIR instrument has not been turned on first, you will
receive an ‘Instrument Failed to Initialize’ warning message on the handheld PC.
If this happens, tap OK, power-cycle the 4100 ExoScan instrument, and restart
the MicroLab Mobile application.

Getting Started
16 Agilent 4200 FlexScan FTIR Operation Manual
2For 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.
CAUTION If a 2.4 GHz cordless phone or a cellular telephone is used near the 4200
FlexScan FTIR, you may experience problems with the wireless communication
and spectroscopic performance. Try turning off the phone or moving further away
from the instrument and attempt the application again.
Performance verification
The 4200 FlexScan 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 below as well as 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 4200 FlexScan FTIR Operation Manual 17
Like any measurement device, it is important to verify that the 4200
FlexScan FTIR is performing properly before using the system to
make critical measurements. The 4200 FlexScan 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 4200 FlexScan. 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 Mobile or 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
18 Agilent 4200 FlexScan FTIR Operation Manual
NOTE When using the external reflectance or grazing angle sample interface, the
appropriate reflectance cap must be in place to make these measurements.
The diffuse gold reference cap should be used with the 45° reflectance
probe when measuring carbon black or other low reflectance samples. The
gold mirror reference cap should be used with the 45° reflectance probe
when measuring thin films or highly reflecting samples. The gold mirror
reference cap should always be used with the grazing angle sample probe.
Table 2. Diagnostic values
Value Optimal (green) Marginal (yellow) Critical (red) Comment
Energy
(centerburst)
29,000
–
21,000 >29,000 or
<21,000
> 31,000 or
< 18,000
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 12,000
–
4,000 >12,000 or
<4,000
>15,000 or
< 3,000
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 4200 FlexScan FTIR Operation Manual 19
Performance validation
The MicroLab PC and MicroLab Mobile software have three tests
appropriate for performance validation of the 4200 FlexScan FTIR.
All of these tests can be accessed from the Advanced Features,
System Check page of the MicroLab PC and MicroLab Mobile
software. The 4200 FlexScan 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. The table below gives the
minimum performance for each sample interface.
Table 3. Minimum performance for the Signal-to-Noise test
Sample interface Specification @ 2500 cm-1 Specification @ 1000 cm-1
ATR 2500 6000
External reflectance 1500 2800
Grazing angle 1500 2800

Getting Started
20 Agilent 4200 FlexScan FTIR Operation Manual
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. For 45 degree external reflectance and
grazing angle reflectance measurements, the appropriate reflectance
reference cap should be in place for the entire test. No reference cap
is needed when using the ATR sample interface. The test results are
expressed as %Transmittance (difference versus 100%) of maximum
deviation during the Stability test. The table below gives the
minimum performance for this test.
Table 4. Minimum performance for the Stability test
Time Specification @ 3000 cm-1 Specification @ 1000 cm-1
30 min 2% 1%