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19 protocols using ftir 600

1

Thermally Controlled FTIR Spectroscopic Setup

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A thermally controlled FTIR spectroscopic system was constructed, as shown in Fig. S1. A spectrometer (FT/IR-4200, JASCO, Japan) was used to obtain the FTIR spectra. A stage (FTIR600, Linkam, UK) was used to control the sample temperature. The sample was inserted between CaF2 plates, and the plates were mounted on a stage with heat-resistant tape. Dry nitrogen gas was passed through the window of the stage to prevent condensation.
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2

In Situ IR Spectroscopy of CO2 Adsorption

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IR spectroscopic
measurements were carried out on the B22 MIRIAM beamline at the Diamond
Light Source using a Hyperion 3000 infrared microscope with a 15×
objective and a liquid N2 cooled MCT detector. The sample
was mounted in a Linkam FTIR600 variable-temperature gas-tight stage
fitted with ZnSe windows, and ZnSe-based linear IR polarizers were
used to obtain polarized IR spectra. Spectra were collected (256 scans)
in the range 650–4000 cm–1 with 4 cm–1 resolution and an infrared spot size at the sample
of approximately 25 by 25 μm. The sample was activated in the
stage prior to measurements by heating at 150 °C under a slow
flow of N2 for 10 h before being transferred to the microscope
and purged under He flow at room temperature. CO2 and
He were delivered to the Linkam stage using separate mass-flow controllers,
the partial pressure of CO2 being controlled by varying
the volumetric flow of the two gases. Both gases were predried through
zeolite filters placed between the cylinders and the mass-flow controllers
before being flowed through the Linkam stage.
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3

Thermal analysis of powder formulations

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HSM observations were made using an Agilent Cary 620 IR optical microscope (Agilent, Santa Clara, CA, USA) equipped with a hot stage (T95 LinkPad and FTIR 600, Linkam, Tadworth, UK). Powder samples of the formulations were mounted on a microscope slide, which was covered with a glass coverslip and placed on the hot-stage furnace inside the sample chamber. The samples were then heated from room temperature to 200°C at a heating rate of 10°C/min. Changes in melting behavior as a function of temperature were recorded as images using Linkam software.
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4

Optical Microscopy Analysis of Crystalline API

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An optical microscope (Agilent Cary 620 IR; Agilent, Santa Clara, CA, USA) was equipped with an electronically controlled hot-stage (T95 LinkPad and FTIR 600; Linkam, Tadworth, UK). Images were collected with and without crossed polarizers to assess the crystalline API content. The samples were heated to 200 °C at a ramp rate of 20 ± 0.1 °C/min and the temperature was maintained until the visual analysis was complete.
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5

Raman Spectroscopy of Samples at Cryogenic Temperatures

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The Raman spectroscopic measurements were conducted on Horiba-T64000 system, coupled with an air-cooled argon ion laser emitting 514.5 nm which is the excitation source. We used LINKAM FTIR 600 cryo-stage is used to collect the Raman spectra at different temperatures in the range 153–300 K. The samples were exposed to laser radiation, using a 50X long distance focusing lens, only during the data accumulation. The Raman data was processed using GRAMS/3 software, and overlapped Raman bands were fitted into several Lorentzian components. The peak position, width and intensity for all the constituents were allowed to vary as free parameters for a convergent fitting.
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6

Thermal Analysis of ARP and Cocrystals

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HSM analysis was conducted with a Cary 620 IR optical microscope (Agilent, Santa Clara, California, USA) equipped with an electronically controlled hot stage (T95 LinkPad and FTIR 600, Linkam, Epsom, Tadworth, UK). The ARP and cocrystal samples were mounted on glass slips, placed on the hot-stage furnace, and heated to 180°C at a rate of 10°C/min. Changes in sample morphology during heating were recorded as images using Linkam software.
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7

Infrared Spectroscopy Analysis of Ion Intercalation

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Bruker Fourier transform infrared spectrometer (Vertex 70 v) integrated with a Hyperion 2000 microscope along with the far- and mid-infrared polarizers were used in the measurement. For mid to near-infrared and far-infrared spectra, the MCT (Mercury Cadmium Telluride) and liquid-helium-cooled silicon bolometer (IR Labs) were employed as the detectors, respectively. Low-temperature measurements were conducted using a cooling and heating chamber (Linkam, FTIR600). The ion intercalation procedure was performed using a lock-in amplifer (Stanford Research 830) and a Keithley 2612B sourcemeter.
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8

Optical Microspectroscopy Analysis of Extrudates

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Optical microspectroscopy studies were performed in reflectance mode by using an Olympus BX41M upright research microscope, equipped with a 50×0.5 NA objective lens. Illumination of the sample was performed with a 30 W halogen lamp. The microscopy setup was equipped with a 50/50 double‐viewport tube, which accommodated a CCD video camera (ColorView IIIu, Soft Imaging System GmbH) and an optical fiber mount. The microscope was connected to a CCD Visible spectrometer (AvaSpec‐2048TEC, Avantes) by a 200 μm core fiber. UV/Vis spectroscopy measurements were performed by using an open in situ cell (Linkam Scientific Instruments, FTIR 600) equipped with a temperature controller (Linkam Scientific Instruments TMS 94). All extrudate samples used in the experiment were of similar dimensions (5×1.5 mm), with spectra collected from approximately 5×5 μm areas of each extrudate. Each sample was impregnated with the desired probe molecule solution (5 μL) at 30 °C, before applying a temperature ramp (at 30 °C min−1) to 120 °C. Optical absorption spectra were recorded every 10 s for a total of 1000 s.
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9

In-situ Confocal Fluorescence Study of Zeolite Catalysis

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Confocal fluorescence microscopy studies were performed with a Nikon Eclipse LV150 upright microscope with a 50×0.55 NA dry objective lens. The confocal fluorescence images were collected with the use of a Nikon-Eclipse C1 head connected to the laser light sources (405, 488 and 561 nm). The emission was detected with three photomultiplier tubes in the range 425–475, 510–550 and 575–635 nm for the three lasers, respectively (in order to avoid channel overlap). Large zeolite ZSM-5 crystals were loaded into an in situ cell (Linkam FTIR 600) equipped with a temperature controller (Linkam TMS 93). The crystals were placed in a flow of 50 mL min−1 O2 and heated to 500 °C at a rate of 15 °C min−1, the crystals were kept at this temperature for 1 h before being cooled to required reaction temperature (at a rate of 15 °C min−1). Once the reaction temperature was achieved, the flow was changed to 50 mL min−1 N2 only. Subsequently, the N2 flow was diverted through a bubbler containing methanol or ethanol for the desired reaction time. The fluorescence intensity was measured across both the middle and surface (top) planes of the zeolite H-ZSM-5 crystals (Figure 2) at varying times under reaction conditions.
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10

In situ UV-Vis Micro-Spectroscopy of Zeolite Catalysts

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The UV/Vis micro-spectroscopy measurements were performed with an Olympus BX41 upright microscope using a 50×0.5 NA high working-distance microscope objective lens. A 75 W tungsten lamp was used for illumination. In addition, the microscope has a 50/50 double viewpoint tube, which accommodates a CCD video camera (ColorView IIIu, Soft Imaging System GmbH) and an optical fibre mount. A 200 μm core fibre connects the microscope to a CCD UV/Vis spectrometer (AvaSpec-2048TEC, Avantes BV). The large zeolite H-ZSM-5 crystals were loaded into an in situ cell (Linkam FTIR 600) equipped with a temperature controller (Linkam TMS 93). The crystals were placed in a flow of 10 mL min−1 O2/40 mL min−1 N2 and heated to 500 °C at a rate of 15 min−1, the crystals were kept at this temperature for 1 h before cooling to required reaction temperature (at a rate of 15 min−1). Once the reaction temperature was achieved, the flow was changed to 50 mL min−1 N2 only. Subsequently, the N2 flow was diverted through a bubbler containing methanol or ethanol for the desired reaction time.
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