PIKE Technologies GladiATR User manual

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Address Comments to:
PIKE Technologies, Inc.
6125 Cottonwood Drive
Madison, WI 53719
Phone [phone]
Fax [phone]
E-mail [email protected]
Web Site www.piketech.com
Jan. 1, 2015

Contents
Introduction
1
GladiATR Assembly View
2
Unpacking Your Accessory
3
Packing List
3
Assembly
5
Installation
7
Accessory Installation
7
Software Installation
8
Installing Videology Image Capture Software
8
Interfacing the GladiATR Vision
8
Installing IC 2.2 Image Capturing Software (BNC)
9
Accessory Alignment
10
Adjusting Camera Focus
11
Performance Verification
12
Sampling Procedures
13
Sample Analysis with High-Pressure Clamp
14
Pressure Clamp Tip Attachments
15
Configuration for Liquid Sampling
16
Configuration for Solid Sampling
18
Configuration for Powder Sampling
19
Crystal Cleaning
19
Effects of Temperature
19
ATR Spectra
20
ATR Correction
21
Useful Equations
22
Solid Samples
22
Crystal ATR Materials
22
Diamond
22
Germanium
22
Precautions
23
Mirrors
23
SAFETY
23
Environmental Ratings
24
Specifications
24
Power Supply Symbol Definitions
25
Replacement Parts and Options
26

PN 350-026019-05 P a g e | 1
Introduction
GladiATR Vision –Diamond ATR with Sample View
The GladiATR Vision™ is a novel sampling tool which couples small area infrared analysis with
simultaneous viewing. Samples are placed face down and positioned on the diamond crystal while its
image is projected in real-time on the LCD screen. Finding and optimizing the sample placement for
specific analysis areas is easy and fast. Analysis of thick or non-transparent samples is no problem
because viewing is through the diamond crystal.
The GladiATR Vision accessory utilizes an innovative optical design with IR beam and visible optical
image converging at the sample position –ensuring that “What you see is what you sample!” The 110X
magnification of the sample image enables the positioning of even relatively small samples into the
center of the diamond crystal for optimized analysis. Analysis of samples as small as 50 microns in size is
possible with the GladiATR Vision accessory.
The GladiATR Vision optical design is all reflective, preserving the full spectral range inherent to
diamond. For standard mid-IR FTIR spectrometers, the spectral range available with the GladiATR Vision
will be 4000 –400 cm-1. For FTIR spectrometers equipped with far-IR optics, the spectral range is
extended to less than 50 cm-1.
Utilizing the diamond crystal of the GladiATR Vision with its 45° angle of incidence the depth of
penetration of the IR beam for most organic samples is about 2 microns at 1000 cm-1. This small depth
of penetration enables most liquid, solid, polymer, gels or paste samples to be measured without any
sample preparation –greatly saving analysis time compared to conventional transmission sampling
techniques. Solid samples are placed upon the diamond ATR crystal, pressure is applied via the click-
stop pressure clamp and the spectrum is collected. Liquid samples are simply applied to the ATR crystal
and the spectrum is collected. If the liquid sample is volatile the optional Liquids Retainer should be
attached to the crystal plate and the Volatiles Cover is placed over the sample before the spectrum is
collected.
Options for the GladiATR Vision include a Ge crystal plate (non-viewing) for high refractive index
samples, a specular reflectance plate (non-viewing) for reflectance analysis of coatings on reflective
substrates and a Flow-Through Attachment.
The GladiATR Vision offers optional resistively heated crystal plates with maximum temperature
operation to 210 °C (diamond) and 130 °C (germanium, non-viewing.) These heated crystal plates are
operated via PIKE Technologies temperature controllers –digital/PC or digital versions.
The GladiATR Vision is available in configurations to fit most FTIR spectrometers.

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Figure 1. Assembly view of the GladiATR Vision ATR accessory
NOTE: High-Pressure Clamp, Liquids Retainer and Volatiles Cover are optional and need to be
ordered separately.
or USB
High-Pressure Clamp
(Optional)
ATR Crystal
ATR Crystal Plate
GladiATR Vision
Base Optics
Baseplate Fastener Screw
LCD, On/Off
Analog Video Output
or USB
Power Input, 12V DC
Brightness,
Higher/Lower
Purge Inlet
Front Panel
(remove to access
alignment screws)
Stainless Steel

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Unpacking Your Accessory
In order for you to quickly verify receipt of your accessory, we have included a packing list. Please
inspect the package carefully. Contact PIKE immediately if any discrepancies are found.
Packing List
GladiATR Vision Manual
GladiATR Vision Base Unit with
LCD Power Cord
GladiATR Top Plate
PN 350-026019
PN 026-19XX
PN 026-2004/5 or 6
Quantity 1
Quantity 1
Must Select
GladiATR High-Pressure Clamp
Pressure Tips
Foam Gaskets
PN 026-3020
PN 025-3099
For Purge Tubes
Optional
One set
Quantity 4
Purge Tubing Kit
Hex Wrenches
Liquids Retainer andVolatiles Cover
PN 025-3055
One set
PN 026-5013
Quantity 1
Optional

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Packing List (Continued)
GladiATR Vision Crystal Plate Options
Description
Part Number
Diamond Vision Crystal Plate
026-2102
Ge Crystal Plate (non-viewing)
026-2050
Specular Reflection Plate (non-viewing)
026-2200
Specular Reflection Plate (viewing)
026-2202
Heated Diamond Crystal Plate, 210 °C, Vision
026-4101
Heated Ge Crystal Plate, 130 °C (non-viewing)
026-4050
The GladiATR base optics assembly has a crystal plate and the purge tubes attached. Some base optics
assemblies may appear different due to specific baseplate mountings for your FTIR.
The pressure clamp, pressure tips, purge tubing kit and wrench set are packed separately in the carrying
case. The purge tubing kit is not needed with most FTIR models. The swivel tip is attached to the
pressure clamp assembly.

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Assembly
1. Attach the GladiATR base optics to its baseplate. This is done by securing the optics base with two
screws, one on each side (Figure2).
Figure 2. Location of screws securing the optics base
2. Install the ATR crystal plate. For proper orientation the serial number is situated at the 1 o’clock
position (Figure 3). The support bar is not visible when using the Ge ATR plate. Installing the ATR
crystal plate improperly will result in no or very low throughput energy through the accessory.
When installing the 210 °C heated diamond plate and the heated Ge plate align the electrical pins on
the plate to the connector pad located on the top of the base optics and continue to follow the
instructions for the standard diamond plate described in step 2.
Serial number
at 1 o’clock position
Front of accessory
Figure 3. Top view of crystal plate properly seated on the accessory

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3. Place the clamp over the dowel pins located on the top of the accessory. Secure using the two large
hex nuts (Figure 4). Instructions for clamp operation are detailed on page 14 of this manual.
4. Complete accessory assembly by pressing the stainless steel top plate over the crystal ATR plate
(Figure 5).
Figure 4. Proper placement of clamp on the Figure 5. Proper placement of top plate over
top of the accessory the crystal ATR plate
5. If purging is required, press the blue tubing included with the GladiATR into the quick-disconnect
port located on the front of the base optics. To remove the tubing, press the black ring of the
opening in and pull the tubing out.
6. For heated configurations, connect the heater cable between the connector (located on the lower
left side of the front panel) and the temperature controller.
7. Connect the video power cable to the right lower front of the base optics.
8. Connect the USB or BNC cable, if the BNC video capture option was purchased, to the lower right
front of the base optics and to the computer (USB version) or frame grabber box (BNC version).
Hex Nut
Hex Nut
Stainless Steel
Top Plate

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Installation
The GladiATR Vision accessory has been aligned and tested in the PIKE Technologies facility on your
model FTIR spectrometer to ensure that it performs to specifications. However, some variation in optical
alignment can occur from spectrometer to spectrometer. To allow for this difference, there are
adjustable alignment screws within the GladiATR Vision base optics assembly for fine-tuning once the
accessory is installed in the spectrometer. The following is the procedure for accessory installation and
final alignment.
Accessory Installation
1. Set your FTIR spectrometer to collect data at 4 cm-1 spectral resolution (including the FTIR J-stop).
2. The GladiATR Vision accessory fits into the sample compartment of the FTIR spectrometer. Your
GladiATR Vision is provided with the appropriate sample compartment baseplate for the model FTIR
instrument you specified. Before inserting the accessory in the sample compartment, ensure that
your spectrometer is aligned. If the instrument is not aligned, maximize the interferogram signal
(the IR energy throughput) of your FTIR spectrometer. This should be performed by following the
manufacturer’s instructions.
3. Fasten the accessory directly into the FTIR sample compartment or onto the FTIR sample
compartment baseplate using the 2 screws located one on each side of the GladiATR Vision base
optics (Figure 1). In order to locate the accessory in the correct position, simply place the entire
accessory into the FTIR sample compartment with the GladiATR Vision label facing the front and line
up the baseplate provided with the holes/pins in your model FTIR spectrometer.
4. Tighten the mounting screws to firmly position the accessory baseplate onto the FTIR sample
compartment baseplate.
5. Mount the pressure clamp onto the back side of the accessory using the two alignment dowel pins
on top of the GladiATR Vision base and fasten using the two hex-head screws into the clamp frame.
6. Install the IC 2.2 software and cables for the BNC version of the GladiATR Vision or Videology
software for the USB configuration. Follow instructions in the next section for your specific
accessory model.

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Software Installation
The GladiATR Vision may be configured for either a USB bus, most often, or a BNC connector. If you have
the USB bus, follow the Installing Videology Image Capture Software instructions. For the BNC
connector, follow the Installing IC 2.2 Image Capturing Software instructions.
Installing Videology Image Capture Software (USB)
Minimum system requirements for the Videology software are a PC with a USB 2.0 compatible port,
Windows XP (service pack 2 preferred) or Windows 7, Pentium 4 2.0 GHz, hard drive speed 5,400 RPM,
and 128 MB of RAM.
Videology CD will automatically launch the installation wizard. If this does not occur, select autorun.exe
file located on the software CD. Be sure the USB cable is NOT connected to the computer USB port at this
time. You will be prompted to connect the USB cable from the Vision to the computer USB port during
installation. After the USB connection wait a few moments for your computer to recognize the hardware.
Additional installation information is located in the Videology manual found on the Videology CD.
Interfacing with the GladiATR Vision
1. With the LCD screen powered on, open the Videology Viewer software. The camera image should be
shown on the computer screen. If the image is not shown, select Advanced Option found under the
Options drop down menu. Check Isochronous Pipe, which determines how the streaming video is
sent through the USB bus. Under the Options drop down menu, select camera settings. The Video
Capture Filter Properties should be set to CVBS as the source and NTSC_M as the format.

PN 350-026019-05 P a g e | 9
2. Prior to capturing images set the folder where images will be saved. From the file menu, select Set
Snap Image Folder and assign a folder. An image is saved by selecting Take Snapshot in the File
menu.
The GladiATR Vision is now ready for alignment.
Installing IC 2.2 Image Capturing Software (BNC)
IC 2.2 is an optional component for the GladiATR Vision that allows the LCD image to be captured and
saved as a .jpg file. To capture saved images, the computer requirements are PC or laptop with PIII/800
MHz/256 MB or higher, a USB 2.2 interface, and Windows XP/SP2, Windows Vista (32 or 64 bit), or
Windows 7 as the operating system.
1. Prior to installing the software, connect the BNC-to-composite video cable to the BNC jack located
on the front of the GladiATR Vision and to the Imaging Source box. Also, connect the USB cable to
the USB 2.0 on the computer and to the Imaging Source box. Then, power up the LCD screen.
2. Follow the Getting Started instructions provided by Image Sourcing for the Video-to-USB Converter
DFG/USB2-It.
3. With the LCD screen powered on, open the IC 2.2 software. Select the DFG/USB2-It drive. The
following settings should be shown on the device bar. With the exception of the FPS (frames per
second), which is a default value depending on the configuration of the computer, the settings
should mimic those shown below - make sure NTSC_M is selected.
4. The LCD image transferred to the computer screen is live. If the image is a still frame, go to the
device menu and select “live” (or press ctrl-l). Image color saturation, brightness, contrast, and
sharpness may be tuned to preference through “properties” found in the device drop-down menu.
5. Images are easily saved by selecting “save image” in the drop-down “capture” menu in either .jpg or
.bmp format. The snap image option in the capture menu will cause the image on the computer to
become still framed; the image on the GladiATR Vision screen remains live. To return to a live image
on the computer screen, select “live” in the device menu or press ctrl-l.
The GladiATR Vision accessory is now ready for optical alignment.

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Accessory Alignment
The GladiATR Vision accessory may not require any alignment when installed - see page 12 for minimum
values. However, should you choose to fine-tune the accessory, follow these steps:
1. Make sure the LCD display is turned off and the power input is removed. Remove the front panel of
the GladiATR Vision accessory by loosening the 4 hex head retaining screws, two on each side of the
front panel. Pull the front panel forward to release from the screws and place it in a secure resting
place on top of the crystal plate on top of the GladiATR Vision base optics (position the High-
Pressure Clamp in the back rotated position to make room for the front panel). Do not undo the
electrical wires connecting the camera and the front panel.
2. Display the live interferogram of the FTIR spectrometer and adjust the input optic, the crystal focus
and the relay mirror. To do this, turn the individual screws one at a time slightly clockwise and check
the signal. If it increases, continue until the maximum signal is obtained. If it decreases, turn the
screw counterclockwise to get the highest possible reading. Follow the order shown in the
alignment image, first adjusting the input optic screw to obtain the maximum signal, then go to
the 2 sets of crystal focus screws and optimize the interferogram signal.
Figure 6. Alignment of the GladiATR Vision
Input Optics
Crystal Focus
Relay Mirror
Do not adjust

PN 350-026019-05 P a g e | 11
3. Finally, adjust the relay mirror screws to optimize the interferogram signal.
4. Repeat the entire procedure 2-3 times to fine-tune the accessory. This is an initial (one-time)
alignment procedure which optimizes the GladiATR Vision to work with an individual optical bench.
Once completed, the alignment does not have to be repeated, unless the accessory adjustments
have been moved or it has been placed in a different FTIR instrument.
You are now ready to verify the GladiATR Vision optical throughput performance.
Adjusting Camera Focus
The camera was focused prior to leaving our facility. You may choose to adjust as clamp pressure may
affect the focusing distance causing a less sharp image. To adjust the camera focus, loosen four hex
screws located on the sides of the front panel, which secure the front accessory panel with the LCD
screen. Remove the front panel to access the focusing thumb wheel. To adjust the camera focus, loosen
the button head screw located underneath the focus thumb wheel. Monitor the image quality while
turning the thumb wheel to the left and right. Only small left or right movements should be required.
Once the optimal focus has been found, tighten the button head screw and secure the front panel with
the 4 hex screws located on the front panel sides.
Figure 7. Camera focus adjustment
Camera Focus Adjustment
Thumb-Wheel
Button Head Screw

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Performance Verification
1. With the accessory removed from the sample compartment, collect an open beam background
spectrum.
2. Place the aligned GladiATR Vision accessory into the instrument.
3. Collect a transmission spectrum using the same collection parameters as used to collect the
background spectrum. This resulting spectrum is termed a throughput spectrum and measures the
IR spectrum of the GladiATR Vision accessory.
4. Place a cursor on the throughput spectrum at 1000 cm-1 and record the value in % transmission.
NOTE: Each of the different crystals (diamond or Ge) will have different looking spectra. An example
throughput spectrum for diamond is shown below. Diamond has strong, broad phonon absorbance
bands in the region of 2100 cm-1. This is normal and will ratio out well in resulting spectra.
The following are the % transmission values the accessory should achieve with different crystal
configurations at 1000 cm-1.
Diamond Crystal Plate: Greater than 14%T
Ge Crystal Plate: Greater than 14%T
GladiATR Throughput

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If your accessory does not meet this minimum transmission level, please contact PIKE Technologies.
Before making this call, please record the serial number located on the label on the back of the GladiATR
Vision base optics assembly.
NOTE: IR throughput performance of your accessory may decrease slowly over time as the ATR crystal
plate surface is exposed to normal wear from cleaning the ATR surface. Please Contact PIKE Technologies
for information about GladiATR Vision service when transmission throughput drops below a usable level.
Sampling Procedures
Collect the background spectrum with the accessory in the sample compartment. Make sure the ATR
crystal is clean and free of any residues. Once completed, place the sample on the crystal surface (apply
the clamp if solid) and collect sample spectrum. A single crystal plate design is used for all types of
samples (liquids, pastes, powders, soft pliable films and solids).
The sample must be in intimate contact with the ATR crystal surface for the evanescent wave to provide
an ATR signal. Note that the Ge crystal used in the accessory is made of materials considerably softer
than diamond. Ge can be scratched if care is not used to remove samples. Scratches on the surface of
the crystal will result in a reduction in the throughput of the accessory. Remove the sample gently with
a non-abrasive cotton tissue and clean with solvent. The crystal plate should be cleaned with an
appropriate mild solvent, such as isopropyl alcohol or a stronger solvent, such as acetone. Cotton swabs
are highly recommended for ease of cleaning without scratching the ATR crystal surface.
Sometimes “carry over” may occur from one sample to another due to incomplete cleaning of a prior
sample from the face of the crystal. This effect may be minimized by collecting a new background
spectrum before each sample spectrum.
Samples should not be left in contact with the crystal for an extended period of time since some samples
may degrade the crystal material and discoloration of the metal plate can occur. Once the measurement
has been made, remove the sample from the crystal and clean the surface of the crystal and the
surrounding plate area with a suitable solvent. Note that the High-Pressure Clamp for the GladiATR can
be swung back to give more access to the ATR crystal area by loosening the smaller clamp knob.

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Sample Analysis with High-Pressure Clamp
1. Loosen the small, arm-securing knob.
2. Raise the clamp arm up and place your sample on the diamond crystal. Some friction during the arm
movement is normal as it prevents its accidental drop and crystal damage.
3. Lower the arm, slightly push the arm-securing knob down and tighten it all the way (please do not
use any tools in this process as finger pressure alone is sufficient).
4. Turn the large clamp knob clockwise to compress the sample. Two “clicks” indicate that the
optimum pressure has been achieved.
5. After the measurement is completed, release the main knob first and the small knob second if the
arm needs to be raised. Please keep in mind that the small knob is spring loaded and it needs to be
pressed in for the screw to engage again.
CAUTION: GladiATR crystal damaged by excessive pressure cannot be covered by the warranty.
Caution is required when using the High-Pressure Clamps with the Ge ATR plate. The diamond crystal
plate is very rugged. This crystal will withstand higher pressures than traditional IR materials, but it still
may be damaged by an excessive force. For this reason, do not exceed the pressure originally set by the
factory on the High-Pressure Clamps. The applied pressure is a function of the size of the pressure tip for
large samples or the size of the sample for small samples.
Main pressure tower knob
Small, arm-securing knob

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Pressure Clamp Tip Attachments
The success of an ATR measurement depends upon the quality of the contact between the sample and
the crystal. Since there is an infinite number of sample shapes and types, a single configuration of the
sample press tip may not be adequate. For this reason, the GladiATR pressure clamp is designed to
accept three different tip attachments, providing the best possible configuration for any given sample
type.
The accessory is shipped with the swivel tip attached to the pressure clamp ordered with the GladiATR
accessory. This tip features an end cap mounted onto a small ball joint. Such design allows the pressure
tip to move and adjust its position to the shape of the sample and maintain the sample position parallel
to the crystal surface. This tip allows for better positioning and optimal contact of thin materials with
the ATR crystal surface. The swivel tip is used with irregularly shaped samples, films, semi-rigid polymers
(e.g. credit card like materials).
The flat tip attachment is a flat-tipped cone and it is used when analyzing thin films, fibers, small
particles, rubber samples and other elastic polymers. The flat tip may also be used for powdered
samples.
The concave tip was developed specifically to work with granules, large beads and polymer pellets. The
tip features a concaved surface which prevents the sample from escaping from underneath the press. It
also forces the spherical samples to stay in the center of the crystal, assuring maximum IR signal
strength. Do not use the concave tip for powdered samples or samples which do not completely protect
the concave edges of the steel tip from pressing against the ATR crystal - this will damage the ATR
crystal.

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Configuration for Liquid Sampling
The crystal plate assembly of the GladiATR accessory features a round plate design with a 3.0 mm
diameter ATR crystal sampling area located in the center of the plate. For liquid sampling, a droplet of
the sample is placed onto the ATR crystal.
For volatile liquids, the optional Liquids Retainer with Volatiles Cover reduces the amount of
evaporation of the sample on the surface of the crystal. To use, place the retainer disk over the ATR
crystal. Place the U-shaped bridge over the retainer disk. Apply pressure to the U-shaped bridge using
the pressure clamp. Fill the reservoir of the Liquids Retainer with the volatile liquid. Slide the Volatiles
Cover between the retainer disk and the U-shaped bridge (Figure 10).
Figure 10. Proper placement of a Liquids Retainer and Volatiles Cover on the GladiATR accessory
For continuous sample monitoring, or for applications where the sample needs to be completely
enclosed for safety or reactivity reasons, an optional Flow-Through Attachment is available. To use,
place the Flow-Through Attachment over the ATR crystal. Apply the clamp to the top of the Flow-
Through Attachment, which creates a seal between the O-ring located on the underneath side of the
Flow-Through Attachment and the ATR crystal plate (Figure 11). Using the Luer-Loc fitting, load the
sample by connecting a syringe or a flow line.
Volatiles Cover
Liquids Retainer
U-Shaped
Bridge
Figure 11. GladiATR with Flow-Through Attachment

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One minute, 4 cm-1 resolution spectra of a dilute detergent solution and distilled water were collected
using the GladiATR Vision with diamond crystal. These samples were applied directly onto the GladiATR
diamond ATR crystal for analysis.
The red spectrum is the detergent solution and the blue spectrum is that for distilled water. A spectral
subtraction can be applied to obtain the spectrum of the detergent component. This is shown in the red
spectrum on the right, and the result will represent the detergent contribution of the liquid sample.
Detergent Solution
Distilled H20
Subtraction Result; Detergent Solution

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Configuration for Solid Sampling
For measurements of soft pliable films and selected solid samples, the sample is placed onto the surface
of the crystal. Since the ATR effect only takes place very close to the surface of the crystal, an intimate
contact has to be made by the sample on the ATR crystal surface. This is achieved by using the pressure
clamp ordered with your GladiATR system. With the sample in place on the crystal, lower the pressure
tip so that it is in contact with the sample. You can continue to turn the pressure knob and increase
pressure to a desired level to obtain a spectrum. However, in most cases, it is recommended to apply
the maximum pressure allowed to ensure the best contact and highest sampling sensitivity. The force
applied by the High-Pressure Clamps is factory set to 40 pounds. The applied pressure is then a function
of the size of the pressure tip for large samples or the size of the sample for small samples. For example,
40 pounds of force upon a sample which completely covers the crystal will generate 6,789 psi whereas
40 pounds of force upon a 1.0 mm diameter flat sample will generate 32,858 psi. The High-Pressure
Clamp has a slip clutch mechanism to avoid exceeding 40 pounds of force.
CAUTION: Care must be used in operating the pressure clamps, since for small hard samples the
maximum pressure may be exceeded.
For the analysis of solid samples the pressure clamp of the GladiATR is required. The sample is placed
face down onto the diamond crystal and force is applied to make intimate contact onto the ATR crystal.
The GladiATR accessory enables us to position the sample to a feature area to ensure that the spectrum
collected is taken from the desired location on the sample. The spectrum below is collected from the
print area on paper. For this analysis pressure was applied to the sample using the swivel tip. The
acquisition time was one minute and the spectral resolution was set to four wavenumber.