Agilent Technologies 4100 User manual

Agilent 4100 ExoScan
FTIR
Operation Manual

2 Agilent 4100 ExoScan FTIR Operation Manual
Notices
© Agilent Technologies, Inc. 2009,
2011-2013, 2017
No part of this manual may be
reproduced in any form or by any
means (including electronic storage
and retrieval or translation into a
foreign language) without prior
agreement and written consent from
Agilent Technologies, Inc. as governed
by United States and international
copyright laws.
Manual Part Number
0023-401
Edition
Sixth edition, October 2017
Printed in Malaysia
Agilent Technologies Australia [M]
Pty. Ltd.
679 Springvale Road
Mulgrave, Victoria, Australia 3170
www.agilent.com
Warranty
The material contained in this
document is provided “as is,” and is
subject to being changed, without
notice, in future editions. Further, to
the maximum extent permitted by
applicable law, Agilent disclaims all
warranties, either express or implied,
with regard to this manual and any
information contained herein,
including but not limited to the
implied warranties of merchantability
and fitness for a particular purpose.
Agilent shall not be liable for errors
or for incidental or consequential
damages in connection with the
furnishing, use, or performance of
this document or of any information
contained herein. Should Agilent and
the user have a separate written
agreement with warranty terms
covering the material in this
document that conflict with these
terms, the warranty terms in the
separate agreement shall control.
Technology Licenses
The hardware and/or software
described in this document are
furnished under a license and may be
used or copied only in accordance
with the terms of such license.
Restricted Rights Legend
If software is for use in the
performance of a U.S. Government
prime contract or subcontract,
Software is delivered and licensed as
“Commercial computer software” as
defined in DFAR 252.227-7014 (June
1995), or as a “commercial item” as
defined in FAR 2.101(a) or as
“Restricted computer software” as
defined in FAR 52.227-19 (June 1987)
or any equivalent agency regulation or
contract clause. Use, duplication or
disclosure of Software is subject to
Agilent Technologies’ standard
commercial license terms, and non-
DOD Departments and Agencies of the
U.S. Government will receive no
greater than Restricted Rights as
defined in FAR 52.227-19(c)(1-2) (June
1987). U.S. Government users will
receive no greater than Limited Rights
as defined in FAR 52.227-14 (June
1987) or DFAR 252.227-7015 (b)(2)
(November 1995), as applicable in any
technical data.
Safety Notices
A CAUTION notice denotes a hazard.
It calls attention to an operating
procedure, practice, or the like that, if
not correctly performed or adhered to,
could result in damage to the product
or loss of important data. Do not
proceed beyond a CAUTION notice
until the indicated conditions are fully
understood and met.
A WARNING notice denotes a
hazard. It calls attention to an
operating procedure, practice, or the
like that, if not correctly performed or
adhered to, could result in personal
injury or death. Do not proceed
beyond a WARNING notice until the
indicated conditions are fully
understood and met.
WARNING
CAUTION

Contents
Agilent 4100 ExoScan FTIR Operation Manual 3
Contents
1. Introduction 5
2. Getting Started 9
Unpacking 9
Packing list 10
Options 11
Components 11
Connecting power 12
Battery 13
AC power 14
Turning on the instrument 18
Power switch LED status 18
Starting the software 19
Charging the handheld PC 20
Logging on to MicroLab Mobile for the first time 20
Performance verification 21
Diagnostic values 22
Performance validation 24
3. Analyzing Samples 27
External reflectance 27
Cleaning the sample probe 29
Collecting a background spectrum 29
Collecting a sample spectrum 30
Internal reflectance (ATR) 32

Contents
4 Agilent 4100 ExoScan FTIR Operation Manual
Cleaning the sample probe 33
Collecting a background spectrum 33
Collecting a sample spectrum 34
Using the solid sample ATR press 36
Interchanging sampling accessories 39
4. Maintenance 41
5. Spare Parts 43
6. Specifications 45
Technical 45
Safety Information 46
Environmental conditions 46
Handheld PC data station 46
Electromagnetic compatibility 47
EN55011/CISPR11 47
ICES/NMB-001 48

Introduction
Agilent 4100 ExoScan FTIR Operation Manual 5
1. Introduction
The Agilent 4100 ExoScan 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 (17.1 x 11.9 x 22.4 cm; 6.75 in x 4.68 in
x 8.81 in), lightweight (3.2 kg; 7 lb) and packaged in a weather-
resistant enclosure suitable for outdoor use. It comes standard with
internal battery power for operation up to 4 hours or can be operated
with 110/220 volt AC power for extended use.
The 4100 ExoScan 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
4100 ExoScan 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 4100 ExoScan FTIR Operation Manual
CAUTION Although the 4100 ExoScan 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 4100 ExoScan 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 4100 ExoScan 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. The various
sampling probes can be provided in a dedicated configuration or with
the capability of being interchangeable. If configured for
interchangeability, the 4100 ExoScan sample probe tips are easily
interchanged in the field by the user. Information on the optimal use
of the different sampling configurations of the 4100 ExoScan system
is listed in the following categories.

Introduction
Agilent 4100 ExoScan FTIR Operation Manual 7
Agilent 4100 ExoScan 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,
chemical degradation of composites and analysis of anodization
of metals. 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. The grazing angle probe is
optimal for analysis of ultrathin films less than 1 micron in
thickness. Specular reflectance is an ideal method for the
analysis of surface contamination. The grazing angle probe
should be used when very low level contamination needs to be
analyzed (nanometer thickness levels). Although primarily
intended as a specular reflectance tool, the External Reflectance
System can also be used for some diffuse reflectance
measurements, which is an ideal method for the analysis of
powders, for example.
Agilent 4100 ExoScan 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 4100 ExoScan 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).
For information about upgrading a dedicated 4100 ExoScan FTIR
system to the capability of interchangeability, contact your Agilent
sales representative or call Agilent directly.

Introduction
8 Agilent 4100 ExoScan FTIR Operation Manual
The 4100 ExoScan 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 4100 ExoScan 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 4100 ExoScan FTIR Operation Manual 9
2. Getting Started
Unpacking 9
Components 11
Connecting power 12
Turning on the instrument 18
Starting the software 19
Performance verification 21
Unpacking
To unpack your spectrometer system:
1After receiving the Agilent 4100 ExoScan 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 4100 ExoScan 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 4100 ExoScan
can be removed and re-packed in the case in a matter of seconds,
while maintaining instrument security.

Getting Started
10 Agilent 4100 ExoScan 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 4100 ExoScan 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. If the optional docking station was
ordered, place the 4100 ExoScan in the docking station.
Packing list
One Agilent 4100 ExoScan FTIR spectrometer system
One Agilent 4100 ExoScan FTIR Operation Manual
One Socket handheld PC system (PDA)
One Agilent 4100 ExoScan FTIR AC power cable
One Agilent 4100 ExoScan FTIR external power supply
One Agilent 4100 ExoScan FTIR USB cable
One Agilent 4100 ExoScan FTIR power/USB ‘Y’ cable
One handheld PC AC power cable
One handheld PC USB cable with power connector
One Agilent 4100 ExoScan FTIR strap
One Agilent MicroLab Software CD
One shipping container

Getting Started
Agilent 4100 ExoScan FTIR Operation Manual 11
Options
Although the 4100 ExoScan FTIR system comes standard as shown
above, there are a number of options available, including:
Laptop computer
Spare USB cable
Extra power adapter
Diamond ATR probe
45° external reflectance probe
Grazing angle external reflectance probe
Diffuse gold reference standard
Gold mirror reference standard
Agilent 4100 ExoScan FTIR docking station
Handheld PC docking station
Components
The 4100 ExoScan 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. The
thumb button can be used to navigate through menu options in the
software.

Getting Started
12 Agilent 4100 ExoScan FTIR Operation Manual
Figure 1.Agilent 4100 ExoScan FTIR
Connecting power
The 4100 ExoScan FTIR can be operated remotely for up to 4 hours
using the 10.8 volt lithium-ion battery, or indefinitely using the AC
power cable when AC power is available. The 4100 ExoScan uses a
single docking style connector for both line power and USB
communication to an external computer. A ‘Y’ cable is included to
connect both the power and USB.
Power on/off button
Handheld PC
data station
Back panel (electrical
connections)
Thumb button (TAB)
Trigger
(RETURN)
Battery door release
buttons (2)
Battery
compartment
Sample probe
interface

Getting Started
Agilent 4100 ExoScan FTIR Operation Manual 13
Battery
The 4100 ExoScan 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 4100
ExoScan should arrive with one battery in the shipping case.
Additional spare batteries are available individually or in
combination with the handheld PC docking station. All batteries
should be fully charged from the factory and ready for use. There is
an LCD display on the front of the battery indicating the level of
charge. Five (5) bars indicate a full charge.
To install the battery:
1Simultaneously depress the button on both sides of the battery
compartment door (see Figure 2).
Figure 2. Battery door release buttons
2Slide the battery into the compartment with the tab of the battery
facing downward and towards the front side of the 4100 ExoScan
FTIR.
3Slide the battery towards the back of the compartment until you
feel the battery engage. There will be a slight resistance when the
battery begins to engage.
Battery door release buttons (2)

Getting Started
14 Agilent 4100 ExoScan FTIR Operation Manual
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 up to four hours on battery power.
To continue using your system while exchanging the battery, you
must have the AC power cable connected between the 4100 ExoScan
FTIR housing and an AC power source.
To remove the battery from the compartment, simultaneously
depress the button on both sides of the battery compartment door
and rotate the door open. Then pull on the black plastic tab to slide
the battery out of the 4100 ExoScan FTIR housing.
It is highly recommended that the battery not be stored in the 4100
ExoScan FTIR unless connected to the main power source for
charging. Similarly to a laptop PC battery, the 4100 ExoScan battery
will slowly discharge when left plugged into the system.
WARNING
Electrical Shock Hazard
Avoid shock hazard. Never allow liquid to run into the 4100 ExoScan FTIR
battery compartment.
AC power
The 4100 ExoScan FTIR is provided with an AC power cord and
external power supply 15 volt DC converter. This can be used to
operate the 4100 ExoScan over extended periods of time or to charge
the 4100 ExoScan battery. The 4100 ExoScan uses a single docking
style connector for both line power and USB communication to an
external computer. A ‘Y’ cable is included for this purpose. Including
the 4100 ExoScan USB cable, there are a total of four cords to make
these connections. In addition, a cable to connect the handheld PC to
USB communication is provided that has a ‘Y’ branch connector to
attach the AC power cord. This AC power is needed for charging the
battery of the handheld PC.

Getting Started
Agilent 4100 ExoScan FTIR Operation Manual 15
To connect AC power to the Agilent 4100 ExoScan FTIR:
1Before connecting the AC power cable to the power source, insert
the 4100 ExoScan FTIR docking style ‘Y’ connector provided into
the connector located at the lower back panel of the 4100
ExoScan spectrometer system (see Figure 3). Next, insert the
power supply cable with the blue female connector into the blue
male connector of the ‘Y’ cable. Thread the blue cap onto the ‘Y’
connector by rotating clockwise until finger-tight. To avoid
damage to the plastic connector, be careful not to over-tighten.
The appropriate power supply cabling will be provided with the
system.
Figure 3.Power connections
CAUTION Use only the included 4100 ExoScan FTIR power supply. Use of other power
supplies may damage the 4100 ExoScan system.
CAUTION The USB connection on the “Y” cable connection is designed to be used with the
4100 Exoscan FTIR at rest; it was not designed for use with the 4100 Exoscan
FTIR in a handheld configuration” to “The USB connection on the “Y” cable
connection is designed to be used with the 4100 Exoscan FTIR at rest only.
Instrument back
panel
Instrument power
cable connector
Instrument USB cable connector
Y cable connection to instrument

Getting Started
16 Agilent 4100 ExoScan FTIR Operation Manual
2Locate the AC power cord and connect to the 15 volt DC
converter box. Then connect 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.
CAUTION Connect the power cord to the spectrometer system first and then to the power
outlet and computer to prevent any power startup damage or problems.
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.
Once AC power is connected, the power button located on the bottom
side of the 4100 ExoScan FTIR handle will appear a solid red color
(see Figure 4). This means the battery pack is being charged, but the
instrument is off.
Figure 4. Power button

Getting Started
Agilent 4100 ExoScan FTIR Operation Manual 17
NOTE The 4100 ExoScan FTIR contains a lithium-ion rechargeable battery pack. Agilent
has fully charged the 4100 ExoScan system prior to shipment, but the system
should also be plugged into a power outlet when not in use. The 4100 ExoScan
battery life under continuous use is approximately 4 hours. It is recommended to
allow the battery pack to be recharged at initial setup prior to turning on the
power to the instrument.
Power cord selection
The following power cords can be used:
Figure 5. Suitable power cords

Getting Started
18 Agilent 4100 ExoScan FTIR Operation Manual
Turning on the instrument
To turn on the instrument:
1Press the power button of the 4100 ExoScan 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 15 seconds. When the LED light illuminates solid
green, the instrument is now ready to use.
2The spectrometer must have a warm up 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 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
Agilent 4100 ExoScan FTIR Operation Manual 19
Starting the software
The 4100 ExoScan FTIR systems are supplied with the Agilent
MicroLab Mobile software, which has already been installed on your
handheld PC computer.
To start the software once the 4100 ExoScan 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 5).
Figure 5. 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
20 Agilent 4100 ExoScan FTIR Operation Manual
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 PC 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 4100 ExoScan FTIR systems are supplied
with the Agilent MicroLab Mobile software already installed on your
system.
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 4100 ExoScan 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.