Non-destructive preserving the integrity of the chemical reaction.In-situ, no extractive sampling required measure chemistry without disturbing the reaction.Real-time measurement, performed every minute or less.The mid-IR energy region yields detailed “fingerprint” spectra of starting materials, intermediates, products and by-products allowing continually tracking of these key species as a function of time.Researchers and scientists improve chemical development by leveraging these advantages, including: In-situ FTIR-ATR offers numerous advantages over alternative analytical methods, including other molecular spectroscopy techniques. With its capability to detect and identify reaction intermediates and measure kinetic parameters, in-situ FTIR is widely used to provide support for proposed reaction mechanisms. In-situ FTIR yields reaction kinetics parameters and defines critical control parameters (CPP) that can be seamlessly transferred to production. This means that rather than running a large number of reactions to understand rate dependencies, just a few experiments can provide the necessary information to determine the driving forces of a reaction.
ESSENTIAL FTIR OFFLINE
In-situ FTIR spectroscopy provides the data to support Design of Experiment (DoE) Studies and other statistical analysis methods without the wait and occasional complex sampling/prep for offline analysis. Data collection is automated, with qualitative or quantitative information typically generated every minute. This technology analyzes batch and flow reactions, reactions in polar and non-polar solvents, and reactions over broad pH, temperature and pressure ranges. In-situ FTIR spectroscopy is widely used in research, early and late development, scale up and reaction optimization. Both diamond and silicon are excellent sensor materials for FTIR-ATR, and the choice of which to use is dependent on the type of chemistry and the infrared peak positions that need to be tracked. Suitable ATR sensors for analyzing chemical reactions must have the requisite index of refraction to enable internal reflection and must also perform in harsh chemical environments without degrading.
The neat solution phase of a chemical reaction is measured and bubbles, particles, catalysts, biological solids, water, etc., do not interfere with the measurement. The restricted depth of penetration of the infrared energy into the sample permits high-quality FTIR spectra of optically dense reaction mixtures. The ATR method is an ideal complement to FTIR instrumentation for analysis and monitoring of chemical reactions. To accomplish this, ReactIR technology uses an internal reflection ( Attenuated Total Reflectance/ATR) sensor mounted at the end of a tubular optical probe that can be inserted into a chemical reaction, or an ATR sensor that is an integral part of a cell monitoring continuous flow reactions. To measure chemistry in real time requires the transfer of modulated infrared radiation into a reaction vessel or continuous flow apparatus, and then the return of the unabsorbed energy to the spectrometer. Additionally, offline analyses can take several minutes to hours for a result, and/ or are susceptible to non-reproducibility. To summarize, all of the above are readily achieved by in-situ FTIR, whereas traditional offline analyses are often impossible to perform (under pressure, highly caustic, air/moisture sensitive, toxic, etc.). With the significant amount of data points collected, in-situ FTIR is highly useful in data rich experimentation, such as Reaction Profile Kinetic Analysis (RPKA). Rates of reaction and other key kinetic parameters are determined from this real-time profiling information, as well as support for proposed mechanisms. Important reaction events are revealed including initiation, steady-state condition and endpoint. Reaction insight comes from identifying and profiling the variations of key reaction species including reagents, intermediates, products and by-products as the reaction proceeds. The capability of in-situ FTIR to provide real-time tracking and monitoring of reaction progress is ideal for developing insight into how reactions work and the means to optimization. Better fundamental insight into how chemical reactions work and the ideal conditions to develop, scale up and operate processes are the key to achieving final product yield, purity and cost objectives. Understanding complex chemical reactions is a major challenge and opportunity for chemists and engineers.