Reaction Monitoring with Reaction View and Reaction Probe

Reaction Monitoring with ® Reaction. View and Reaction. Probe™ In-situ contamination and surface analysis with Spot. View and Spot. View-SL © Remspec Corp. 2014

Remspec Corporation Remspec has been manufacturing and selling mid-IR fiber optic systems since 1993 (over twenty years). We have sold hundreds of fiber-optic probes and systems to academic and industrial customers all over the world. We have more experience with mid-IR fiber optics than any other company and we make the fiber in-house. Our software is designed by synthetic chemists to be used by chemists and we can provide fully customized software. Our experienced scientific staff provides full support for applications development, including calibration development. © Remspec Corp. 2014

Reaction. View® Range 900 -5000 cm-1 ATR and transmission heads fit wide range of reactors Full control and display software on a laptop 20 hr detector dewar for overnight experiments © Remspec Corp. 2014

Reaction. Probe™ Remspec's probes can be used with most commercial FTIR units. The signal is taken from the sample compartment to the probe, and returned from the MCT detector to the spectometer. All of the interchangeable heads are available with the Reaction. Probe. © Remspec Corp. 2014

Modular Systems Remspec systems are fully modular: Analysis heads for high or low temperature, high pressure, corrosive solvents. Replaceable ATR crystals for standard conditions, high and low p. H, corrosive conditions. Liquid transmission head for very low concentrations Short-path gas transmission cell. Only the head is changed for changing conditions or different types of reactor port. ATR and transmission crystals are replaceable and Remspec offers low-cost rebuilding of fiber-optic probes for low total cost of ownership. © Remspec Corp. 2014

ATR Head • A range of materials can be used (Zn. Se is shown) • Good, general-purpose probe • Sensitive down to about 0. 1 wt. % of most analytes • Works in all solvents, including water • Stainless steel* probe, shaft Kalrez® seals, and inert crystal materials make the probe corrosion-resistant. • The room-temperature head is shown. *Hastelloy is available for extreme conditions © Remspec Corp. 2014

Transmission Head The Liquid Transmission Head lowers the detection limit to <0. 1 m. M. It is a double-pass transmission cell with a mirror wall. It can only be used in solvents that have low mid. IR absorbance (e. g. hexane, acetonitrile, methylene chloride, THF); suspended solids can interfere with performance. © Remspec Corp. 2014

Analysis Heads: High Temperatures High Temperature Head Gas cooled (air or nitrogen) ATR or Transmission -100ºC to >200ºC 15 mm OD Available with chemically resistant polymer end for low heat transfer © Remspec Corp. 2014

In-Situ Spectroscopy at High Pressures High Pressure Head (example) Custom seal (cone in cone fitting shown) ATR or Transmission Pressure to 200 bar Cooled (air or nitrogen), -100ºC to >200ºC (standard) Water and gas cooled -100°C to 300°C (special order) © Remspec Corp. 2014

Viz. IR™ Software Available with Reaction. View Can collect a single dataset for 3. 5 days at one spectrum per minute (5000 spectra) Viz. IR includes a Control Panel for setting the resolution and timing of data collection during an experiment, as well as Start and Stop buttons. The display windows show a 3 D picture of the spectra versus time, and a window for most recent spectra or trend-lines. PCA/ITTR analysis with Reaction. Sleuth™ © Remspec Corp. 2014

Example: 2 -step Organic Synthesis 2 -step commercial synthesis reaction Step 1 Anion formation Step 2 Product formation Solvent is DMF Note solvent peak at approx. 1400 cm-1. © Remspec Corp. 2014

Reaction Monitoring in Summary Remspec manufactures and supplies mature, well supported systems with a wide choice of sampling options that are easy to use and provide repeatable data. Remspec provides specialized software that is optimized specifically for reaction monitoring and the analysis of reaction data. © Remspec Corp. 2014

Grazing Angle FTIR Spectroscopy © Remspec Corp. 2014

Spot. View Head Hand-held grazing angle unit Sensitive to <1 μg/cm 2 Suitable for large flat and curved surfaces Works on metal, glass, and most plastics © Remspec Corp. 2014

Spot. View Case Study: inside stainless steel production tanks Tank interior (agitator shaft of CIP system). Note: spectral features in top trace, eventually identified as residue from cleaning material, traced back to pump used in cleaning cycle. Baseline shift, characteristic of contaminated surface © Remspec Corp. 2014

Spot. View-SL Head • Hand-held direct reflectance unit • Sensitive to ~3 μg/cm 2 • Suitable for small curved or low-access surfaces • Works on metal, glass, and most plastics © Remspec Corp. 2014

Spot. View-SL Case Study: polymer residue on steel extrusion screw Upper trace: 3. 5 μg/cm 2 Integration: 0. 19 Lower trace: 6. 0 μg/cm 2 C-H stretch feature is integrated. A PLS 1 calibration can also be built. Integration: 0. 30 © Remspec Corp. 2014

Surface Analysis in Summary Remspec manufactures and supplies both grazingangle and direct reflectance heads for flat and curved, large and small surfaces. Remspec provides: specialized software that can be set up for “push-button” use by the operator. Calibration development and support services. © Remspec Corp. 2014