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INSTALLING YOUR REACTIONPROBE ACCESSORYSYSTEM ON A BRUKER
FTIR
1 Unpacking
The ArtView accessory is shipped in a custom box. We recommend
that you keep the box, in case you need to store the ReactionProbe
or ship it. When you open the box, take out the top layer of foam,
lift the fiber-optic cable carefully and place it gently on a flat
surface where it will not fall, and where heavy objects will not be
placed or dropped on it. The smallwhite funnel that is packed
beside it is for use with the detector.
The ReactionProbe probe in the shipping box.
Do not bend the cables any more than this, and handle the probe
gently.
The funnel is used to add liquid nitrogen to the detector.
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The external MCT detector is packed below the second layer of
foam.
The MCT detector is housed in its own box, with a liquid
nitrogen inlet on top of the dewar, and an optical connection on
the side of the box.
We recommend placing the detector box on top of the FTIR if
possible.
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The In-Compartment Fiber Launch Module ispacked in a slot in the
second layer of foam, next to the Detector Unit.
[If your system includes an external detector, you will have one
Launch Module; if there is no external detector, you will have two
Launch Modules.]
A power cable for the detector unit and a signal cable to
transfer the FTIR signal from the detector back to the FTIR are
also included.
• If any components are missing or appear to be damaged• If you
have any questions or concerns
Please contact Remspec before proceeding with the installation
and set-up.
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2 Installing the Fiber Launch Module in the
SampleCompartment
The In-Compartment Fiber Launch Module (Fig 1) comprises a
mirror and a three-axis positioner assembly. The three adjustments
(x,y,z) are locked with four bolts and a locking nut (all silver
colored). It fits into the slide-mount in the FTIR sample
compartment (Fig 2).
Figure 1: the In-Compartment Fiber Launch Module
Figure 2: the slide-mount bracket in the sample compartment of a
Bruker Vector 22 spectrometer
Figure 3: slide the in-compartment optical launcher into the
fitting.
Figure 4: Make sure that the launcher is fully seated in the
mount.
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Note about Mirrors:IR radiation entering the sample compartment
is collected by a mirror and focused onto the end of the mid-IR
cable held by the in-compartment launcher. It is important that
this collection mirror remain clean. Since it is enclosed, the
build up of dirt, dust, or scratches isminimized. If cleaning is
required, a gentle stream of dry, oil-free air or nitrogen should
be directed at the mirror. DO NOT CLEAN THE MIRROR WITH ANY TISSUE
OR CLOTH.
Figure 5: The fiber-optic probe should be setup in a clamp stand
so that the shaft is vertical. Handle the fiber-optic bundles very
carefully. A metal mirror is needed for testing; it is recommended
to place it on a laboratory jack so that it can be raised and
lowered.
Figures 6 & 7: Take the longer fiber-optic cable (it has 7
fibers in it) and position the end of it above the screw fitting on
the in-compartment launcher. Gently fit it into the center of the
fitting, then screw the black nutinto place. Be careful not to
loosen the silverlocking nut.
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3 Installing the Detector Module
We recommend placing the detector module on top of the FTIR unit
if possible. Make sure that it is in a stable position.
If you have an in-compartment fiber launch module, you should
position the detector so that the two fiber cables can reach the
detector and the launch module without twisting or stretching.
The signal cable has two different connectors.One is a Lemo
connector. It should be inserted into the socket on the back of the
detector box. Make sure that the red dot on the connector is lined
up with the dot on the socket.
The other connector on the signal cable is a 15-pin D connector.
It must be inserted into one of the external detector ports on the
FTIR.
Make sure that your system, and your OPUS software, is set up
for an external detector.
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Before using the system, remove the lid from the red dewar, and
use the white funnel to fill the dewar with liquid nitrogen. Wear
safety glasses when handling the liquid nitrogen, and pour it
slowly.
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3 Attaching Mid IR Cables to the Fiber Launch Module &
Detector Module.
The Remspec Mid-IR Fiber Optic Probe (Figure 11) consists of a
stainless steel shaft with an attached sampling head and two
fiber-optic cables for attachment to the Launch and Detector
modules. The longer cable, which comprises seven fibers, should be
connected to the launch module by holding the ferrule at the end of
the cable and gently sliding it into the ferrule holder of the
three axis positioner (Figure 10). Be careful not to bang the ends
of the cable against the ferrule holder! (See section 2.3 of the
Remspec Manual for handling information). Once the ferrule is well
into the ferrule holder tighten down with the ferrule nut (Figure
11). If you intend to remove the cables for storage, make sure the
ferrule nut is not too tight. Repeat this process to attach the
shorter cable (comprising twelve fibers) to the three-axis
positioner on the Detector module.
The fiber-optic probe should be set up in a clamp stand so that
the shaft is vertical. Handlethe fiber-optic bundles very
carefully. A metal mirror is needed for testing; it is recommended
to place it on a laboratory jack so that it can be raised and
lowered.
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The longer (7 fibers) fiber-optic cable should be connected to
the launch module.Position the end of it above the screw fitting
onthe in-compartment launcher.
Gently fit the cable end into the black ferrule-holder, then
screw the nut into place. Be careful not to loosen the
silver-coloured locking nut.
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4 Testing the ReactionProbe
To test the probe, or to collect a background spectrum before
collecting data, a metal mirror is required. A gold-coated mirror
or polished stainless steel can be used (the steel is easier
toclean).If you use a reflectance head, it must touch the surface
of the mirror very gently to give the correct spacing. You can then
use OPUS in the usual way to check the signal and collect a
background.If you do not have a reflectance head, or need to use
the probe without any contact on the background or the sample, the
probe must be positioned about 3-4 mm above the mirror to check the
signal.
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5 Installing High-Temperature Analysis Head
The high-temperature ATR head can be used at temperatures
between -100° and +200°C. Cooling gas is required for use above
60°C, and the cooling gas should be chilled for use above 120°C.
Control the cooling gas flow to keep the thermocouple temperature
below 40°C (a temperature read-out is supplied; the thermocouple is
already installed in the head, do not remove it).No cooling is
required if the fiber probe is removed. This means that the
analysis head can be sterilized along with the reactor so long as
the fiber probe is removed.It is important to secure the ATR head
into the required position in the reactor BEFORE attaching the
fiber-optic probe. The head should be carefully inserted into the
reactor port and supported (e.g. with a clamp) in the desired
position. The head may be secured into a compression fitting (e.g.
Swagelok). Do not over-tighten.Insert the fiber-optic probe into
the head and secure it BEFORE attaching the cable ends to the FTIR
and to the detector.
To install the high-temperature head:1. Loosen the set screw2.
Gently slide the head onto the probe
shaft as shown until the probe end contacts the ATR crystal.
3. It is important to move the fiber-opticprobe carefully
without stretching or bending the cables.
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To secure the head:1. When the probe end contacts the
crystal, carefully stretch the spring byabout 5 mm.
2. Tighten the set screw to hold the head in place.
3. Make sure that the fiber-optic cables are not stressed.
4. If cooling gas is required, attach the gas hose to the hose
barb. When gas is flowing, it will leave the head by the Gas
Exit.
5. Finally, connect the fiber-optic cablesto the FTIR and the
detector, and check the signal level in the FTIR software. You can
carefully rotate thehead by up to 1/2 turn to maximize the
signal.
Notes:• Cooling gas (dry nitrogen or “instrument air”) is
required only if the reaction will
run above 60°C.• Cooling is required only when the fiber-optic
probe is in the head.• The head can be left in place without
cooling when the reactor is sterilized if the
fiber-optic probe is removed.• When using the high-temperature
head, we recommend using an air background.
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INSTALLING YOUR ReactionProbe accessory system ON A BRUKER FTIR1
Unpacking2 Installing the Fiber Launch Module in the Sample
Compartment3 Installing the Detector Module3 Attaching Mid IR
Cables to the Fiber Launch Module & Detector Module.4 Testing
the ReactionProbe5 Installing High-Temperature Analysis Head