Keit IRmadillo DOC1049R User manual

DOC1049R
22 February 2024, 12:07
DOC1049R IRmadilloNA User
Manual - Hardware
Model Number: ASM0627-09-N-Cx-O-Gx-D3x
www.keit.co.uk
[email protected]

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Table of Contents
1.1. Purging the IRmadilloNA.........................................................................................2
1.2. Avoiding fouling ......................................................................................................3
1.3. Checking for warnings and checking the probe is clean..........................................5
1.3.1. Cleaning instructions........................................................................................5
1.3.2. Recognising if the probe is clean .....................................................................6
1.4. Taking a background ..............................................................................................7
2. Maintenance..................................................................................................................8
2.1. Spectrum health......................................................................................................8
2.1.1. Use at high temperature ..................................................................................8
2.1.2. Emitter ageing..................................................................................................9
2.2. Remote health check..............................................................................................9
2.3. Cleaning the fibre optic data cable connectors........................................................9
2.3.1. Cleaning the Souriau fibre-optic connectors...................................................10
3. Components ................................................................................................................13
3.1. Storage conditions................................................................................................13
4. Accessories .................................................................................................................14
4.1. Sample cell - ASM1398 ........................................................................................14
4.1.1. Maintenance..................................................................................................14
4.1.2. Cleaning ........................................................................................................14
4.2. Flow cells..............................................................................................................15
4.2.1. High flow cell - ASM1392...............................................................................15
4.2.2. Low flow cell - ASM1222................................................................................16
4.3. Inclined Stand –ASM0916....................................................................................18
4.3.1. Safety............................................................................................................18
4.3.2. Installation .....................................................................................................19

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This document should be read in conjunction with DOC1048R IRmadilloNA User Manual –
Safety.
1.1. Purging the IRmadilloNA
The IRmadilloNA spectrometer is designed to be continuously purged. This eliminates any
interference in operationcaused by changing levels of water vapour and carbon dioxide (CO2)
within the instrument, both of which interact strongly with infrared (IR) light.
The IRmadilloNA is fitted with purge inlets on the probe and spectrometer body. The Inlets are
shipped with blanking plugs that need to be removed before use. There are breathers on both
the probe and spectrometer body.
Figure 1: Purge inlet and outlet locations on ASM0627-09
The ideal purge gas is dry nitrogen. Alternatively, dry air from a purge gas generator can be
used. The output from this purge gas generator should have a minimum quality according to
ISO8573-1:2010 of Class 1:2:1 (dust:water:oil) or better. Keit can recommend suitable
generators that achieve this outlet air quality; contact suppo[email protected]. Purge gas
generators may include an internal compressor or use factory-supplied compressed air with a
minimum quality of Class 4:4:4 (dust:water:oil).
NOTE
REMARQUE
All FTIR spectrometers are very sensitive to water vapour and
carbon dioxide. Even in well-controlled environments, e.g.,
laboratories, environmental changes can be large enough to
cause significant changes in the spectrum. We STRONGLY
recommend purging the instrument at all times.
Tous les spectromètres FTIR sont très sensibles à la vapeur d’eau
et au dioxyde de carbone. Même dans des environnements contrôlés
(des laboratoires, par exemple), les changements dans
l’environnement peuvent être suffisants pour causer des variations
de spectre significatives. Il est VIVEMENT recommandé de toujours
purger l’instrument.

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To purge the instrument:
•Remove the blanking plugs from the gas purge inlets on the instrument probe and
body; these are push fit connectors.
•Connect either a 4mm or 5/32” diameter stainless steel or PTFE hose to the purge inlet
ports.
•Ensure the gas tubes are connected to a suitable gas supply via a flow meter (we
recommend 1 adjustable flow meter per instrument)
•Adjust the total flow to 0.5 - 2 litres per minute (The pressure drop through the unit is
<1 barg).
•Do not turn off the purge during normal operation; this will impact the instrument’s
performance.
•If the purge tubing is disconnected, the blanking plugs must be fitted to the inlet
connections on the probe and body to maintain the IP rating and exclude dust.
The IRmadilloNA requires a stabilisation period of >12 hours once powered on and purging
has started. This is to allow the internal components to reach a stable temperature and
complete purging. Once fully purged the instrument is very robust against changes in ambient
conditions, provided the purge gas supply is maintained.
1.2. Avoiding fouling
The diamond window at the tip of the probe must be in contact with process fluid to give a
measurement. Even a thin layer of scaling or fouling will prevent the IRmadilloNA from being
able to ‘see’ the process fluid.
To minimise the risk of fouling of the diamond window, we recommend taking the following
steps during installation:

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Figure 2: Installing the IRmadilloNA in a fouling environment.
1. Particularly for continuous processes, install the IRmadilloNA in a bypass loop which can
be isolated using valves A and B. This makes it easy to retract the IRmadilloNA for manual
cleaning if required without the need to interrupt the process flow.
2. Direct the flow through the IRmadilloNA’s bypass loop by blocking or restricting the ‘main’
flow unless the bypass loop is to be isolated (valve C). Alternatively, this may be achieved
by mounting in a pump bypass loop (offtake from pump discharge and return to pump
suction).
3. Maximise theflow velocity pastthe IRmadilloNA by installing in areduced-diameter section
of the pipe. The minimum flow velocity should be 1.5 m/s (5 ft/s).
4. Install the IRmadilloNA so that the probe tip is fully in the flow. We recommend putting the
probe tip as close to the centre of the pipe as possible.
5. The direction of flow should be vertically upwards. This both minimises the risk of air
bubbles becoming trapped around the probe tip and reduces the risk of settling of any
sediment that is present.
6. To increase the pressure, install the IRmadilloNA after a pump. Higher pressure minimises
the risk of sedimentation and bubbles.
7. Where possible, install the IRmadilloNA at a location where the process conditions are
less prone to fouling. Depending on your process chemistry, this may be achieved by
choosing a high temperature location and using heat tracing and insulation to avoid
localised cooling. Higher process temperatures often maximise the solubility of potential
fouling substances.

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8. Fit ports either side of the IRmadilloNA’s install point to allow clean-in-place or flushing
with a suitable cleaning fluid.
1.3. Checking for warnings and checking the probe is clean
When you have connected to the powered-on IRmadilloNA the KeitSpec application should
load automatically (within 3 minutes). It is important to confirm that the system is working
without errors: information on IRmadilloNA warnings and errors can be found in DOC0893
KeitSpec Software User Manual, section 1, Getting Started.
Once the system is set up without errors, the probe tip must be cleaned, and a background
spectrum must be taken before insertion into the vessel or pipe. If the probe is guaranteed
clean, the factory background scan shipped with the instrument –and saved to the desktop of
the controller –can be used. Cleanliness of the probe tip is important to performance; if you
suspect fouling or scale build-up, perform a clean appropriate to your environment.
1.3.1. Cleaning instructions
Rinse the ATR element with a suitable solvent. The choice of solvent will depend on your
process. You may fully immerse the ATR in solvent if needed. The following are suitable:
•Water
•Acetone
•Alcohols
•Surfactant solutions
•Alkanes (hexane, cyclohexane etc…)
•Ethers
Once exposed to a suitable solvent, wipe the ATR with a clean cloth. The metal tube of the
probe can also be cleaned by wiping with a cloth.
For hard-to-remove fouling (such as biofilms or dried-on chemicals) Keit recommends an
oxidative acid clean. First, clean the ATR using the methods outlined above, then perform the
following: Souriau in-line plug
•If you have purchased one, place the PTFE sample cell on the end of the probe and
fill with ~4ml of 1 M nitric acid solution. If you have not purchased one then please
contact [e-mail] for further information.
•Leave to soak for 1 hr
•Carefully remove the acid using a pipette and fill the sample cell with water
•Remove the water using a pipette
•Remove the sample cell and rinse the ATR again with water
•Carefully wipe the ATR with a cloth
It may be necessary to repeat the cleaning steps again if the contaminant has only been
partially removed.
In some cases, it may be necessary to perform an alkali clean on the probe. First clean the
ATR using the methods outline above, then perform the following:
•Place the PTFE sample cell on the end of the probe and fill with ~4ml of 1 M sodium
hydroxide solution
•Leave to soak for 1 hr
•Carefully remove the alkali using a pipette and fill the sample cell with water
•Remove the water using a pipette

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•Remove the sample cell and rinse the ATR again with water
•Carefully wipe the ATR with a cloth
It may be necessary to repeat the cleaning steps again if the contaminant has only been
partially removed.
1.3.2. Recognising if the probe is clean
When looking to see if the instrument is clean, the primary area of interest within the spectrum
is between 800 and 1800 cm-1. This section ofthe absorbance plot shouldmaintain a relatively
flat line with no consistently repeating peaks. Cleaning Mode can be used to see the effects
of the cleaning process in real time –see DOC0893 KeitSpec Software User Manual, Section
2, The Spectrometer Tab.
Figure 3: A clean probe showing no significant peaks within the 800 to 1800 cm-1 region.
Several sharp peaks in the region 800-1800 cm-1 indicate that the probe has not been cleaned
properly.
Figure 4: Sharp spikes within the region indicating an unclean probe

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A peak at 1400 cm-1 indicates that there is some water on the probe. This could indicate poor
purge quality.
Figure 5: Peak indicating the water in the spectrum
A negative peak indicates that although the probe is clean now, it was not clean when the
background was taken. Another background must be taken before any spectra can be
measured.
Figure 6: Negative peaks indicating the background was taken when the probe was unclean or not fully
purged.
1.4. Taking a background
FTIR requires the collection of a background spectrum (also called a reference or baseline
scan) before any absorption scans can be performed. This must be performed before the
probe is inserted into the reaction/process of interest. The process for collecting a reference
scan can be found in DOC0893 KeitSpec Software User Manual, Section 1, Getting Started.

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2. MAINTENANCE
Probe accessories may contain O-rings, which we recommend replacing annually or, where
worn or damaged, more frequently. See Section 4 Accessories for more information on
accessories.
2.1. Spectrum health
The spectrum can be used as a good indication of the health of the instrument.
2.1.1. Use at high temperature
Figure 7: Probe is heated causing the spectrum to tilt
In Figure 7, the spectrum is tilted, with positive absorbance at lower wavenumbers and
negative absorbance at high wavenumbers and the spectrum is not flat in the region 800-
1800cm-1. This indicates that the probe tip is at a higher temperature now than it was when
the background was taken. This may cause chemometric models to give incorrect results
unless the model uses an appropriate pre-treatment to remove the effect. Any model built by
Keit will have this taken into account.

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2.1.2. Emitter ageing
Figure 8: Spectrum is tilted showing signs of emitter ageing
The infrared emitter in the probe is expected to age over its lifetime. The results of this can be
seen in Figure 8: the spectrum is tilted; the absorbance is positive across the whole spectrum;
and the spectrum is not flat in the region 800-1800 cm-1 (contrast with Figure 3, above). If
evidence of emitter ageing is seen, it may be required to take a new background scan to
remove this effect –contact Keit for advice.
2.2. Remote health check
Keit can perform an annual examination of your system’s health data remotely to determine if
any servicing needs to be carried out. This includes review of internal diagnostics for warnings
and errors, component performance for signs of premature ageing, and evaluation of
background reference spectra history for signs of operator error or progressive damage.
Remote health checks are offered annually as a part of our MSP.
2.3. Cleaning the fibre optic data cable connectors
Once installed and in normal operation there should be no need to clean the fibre optic
connectors. If the instrument needs to be moved so the connectors are disconnected, it is
recommended that the connectors are cleaned before being re-connected.
The fibre connectors are cleaned with a cleaning pen as shown below.
Figure 9: Fibre-cleaning pen