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2012 Corporate Capabilities - Spectroscopy

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www.spectroscopyonline.com<br />

December 2011 <strong>Spectroscopy</strong> 26(12) 21<br />

Temporary Online FT-IR<br />

<strong>Spectroscopy</strong> for Process<br />

Characterization in the<br />

Chemical Industry<br />

The focus of this paper will be on the use of temporary online Fourier-transform infrared<br />

(FT-IR) spectroscopy in the chemical industry including two case-study applications involving<br />

fouling and product quality. These case studies will be followed by a discussion of the use of<br />

temporary online FT-IR analysis enabling process optimization.<br />

Serena Stephenson, Lamar Dewald, Esteban Baquero, Wendy Flory, Liane Mikolajczyk,<br />

and J.D. Tate<br />

The Dow Chemical Company (Midland, Michigan)<br />

is the world’s largest integrated chemical company<br />

utilizing a wide variety of unique chemistries in<br />

the production of both basic and specialty chemicals.<br />

The diversity of chemical processes and the interrelationships<br />

of production facilities in the integrated chemical<br />

complex provide significant opportunities for process<br />

optimization. Fouling, corrosion, plugging, or out-ofspecification<br />

product occurrences in one manufacturing<br />

plant can have negative effects on the operation of one<br />

or more downstream facilities. Accurate and representative<br />

data for process characterization is a key factor in<br />

making informed decisions regarding the resolution of<br />

process problems. The information-rich nature of optical<br />

spectroscopy and, in particular, Fourier-transform infrared<br />

(FT-IR) spectroscopy is uniquely suited for rapid and<br />

continuous online process characterization.<br />

Sometimes grab samples of the process that are analyzed<br />

in the laboratory provide sufficient data for process<br />

characterization. However, the nature of a process<br />

stream frequently makes collecting representative grab<br />

samples difficult. Gas-phase samples, reactive samples,<br />

and samples under elevated (or depressed) temperature<br />

or pressure are a few examples of samples that are particularly<br />

difficult to collect and analyze by laboratory<br />

analysis. Streams where trace (for example, low parts per<br />

million) levels of water or carbon dioxide are the analytes<br />

of interest are also a particular challenge for grab<br />

sample laboratory analysis because concentration levels<br />

are easily influenced by atmospheric composition. Safety<br />

issues must also be considered when collecting samples<br />

of highly toxic or explosive materials such as phosgene,<br />

acrylates, ethylene oxide, hydrogen chloride, or isocyanates.<br />

Depending on the duration and extent of required<br />

toxic material analyses, properly designed continuous<br />

online analysis can help mitigate associated safety issues.<br />

Additionally, when the process event of interest is<br />

transient occurring over a short time-frame, occurring<br />

at unknown intervals, or if the process is not at steadystate,<br />

a continuous online analysis of a representative<br />

sample provides a richness of insight into the process<br />

that would not be achievable by the infrequent glimpses<br />

into the process that is attainable by grab sample analysis.<br />

Lastly, continuous analyses are an invaluable tool<br />

during new process development and process scale-up<br />

due to the ability to thoroughly characterize the process.<br />

Of the available analytical tools for temporary online<br />

process characterization, FT-IR is among the most powerful.<br />

FT-IR is a fast technique providing fundamental<br />

vibrational information for the components in the stream<br />

and allowing the capture and retention of informationrich<br />

spectra. The raw data obtained from FT-IR are often

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