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