Monitoring, NIRS analyses products

A further example of process quality monitoring and reactor batch profiling using NIRS comes with oleo-chemical and biodiesel production. An established use of FT-NIR analysis (AOCS Method Cd le 01) is the determination of the key vegetable oil processing parameters - iodine value (IV) and percentage trans fat content (%Trans) (Figure 5.38). 

The NIR spectrometer used for method development and sample analysis was a Foss NIR Systems Model 6500 Forage Analyzer with a sample transport module and a standard reflectance detector array. The transport module moves the sample compartment up and down during data collection, thereby allowing a more representative spectrum to be obtained from bulky heterogeneous samples. The reflectance array uses two silicon detectors to monitor visible light from 400-850 nm and four lead-sulfide detectors to monitor NIR light from 850-2500 nm. Natural product sample compartment cells in 1/4-cup and 1-cup sizes were used as sample holders in the transport module. This instrument has a maximum resolution of 2 nm. 

Several resin producers have considered programs for the introduction of on-line NIR analysis into their production facilities, i.e. process control of additive dosage. NIRS has been used to monitor polymer melts for polymer and/or additive composition with in situ analysis in transmission, trans-flectance and reflectance modes. Research on the application of NIRS to in-line and on-line additive analysis in melts (Table 7.21) is as yet by no means as extensive as in case of UV (Table 7.15) and mid-IR (Table 7.17). Batra etal. [143] have applied NIRS... 

IR is one of three forms of vibrational spectroscopy that is in conunon use for process analytical measurements the other two being near-lR (NIR) and Raman. Each one of these techniques has its pros and cons and the ultimate selection is based on a number of factors ranging from sample type, information required, cost and ease of implementation. The sample matrix is often a key deciding factor. NIR has been the method of choice for many years within the pharmaceutical industry, and sample handling has been the issue, especially where solid products are involved. IR is not particularly easy to implement for the continuous monitoring of solid substrates. However, often there is no one correct answer, but often when the full application is taken into account the selection becomes more obvious. In some cases very obvious, such as the selection of IR for trace gas analysis - neither NIR nor Raman is appropriate for such applications. 

Carl Zeiss, Inc. also describes a spectrofluorometer system for process monitoring," but it does not currently appear as a standard marketed product on their web site. HORIBA Jobin Yvon also markets a fluorescent process analyzer, but it is a laser-induced time-domain based measurement system tailored for uranium or equivalent analysis." Finally, while numerous miniature spectrofluorometers are also available (Carl Zeiss, StellarNet Inc., Ocean Optics and Avantes), they are not packaged and configured for process applications. Although there is an established need and continued growing interest in realtime process spectrofluorometry, relative to conventional process spectroscopic instruments such as NIR, UV-vis and Raman, commercial process spectrofluorometers are currently available on a very limited basis. 

First and most importantly, real-time NIR monitoring enabled real-time control of the process. For a given product, the molecular weight and end-group balance in the prepolymer exiting the front end or melt part of the process must be controlled at specified levels in order for the back end or solid-phase part of the process to successfully produce the intended polymer composition. In addition, the variability in prepolymer composition must be controlled with very tight tolerances to keep the variation in final product composition within specification limits. Since the process dynamics in the front end were more rapid than those in conventional PET processes, the conventional analytical approach involving off-line analysis of samples obtained every 2-A hours was not sufficient to achieve the desired product quality. 

NIR spectroscopy is a popular method for qualitative and quantitative analysis. It is finding widespread use in many different industries for monitoring the identity and quality of raw materials and finished products in the food, agricultural, polymer, pharmaceutical, and organic chemical manufacturing industries. 

On-line MIR ZnSe ATR analysis of microbial cultures has been used primarily for non-invasive monitoring of alcoholic or lactic fermentations. Alberti et al. [76] reported the use of a ZnSe cylindrical ATR crystal to monitor accurately substrate and product concentrations from a fed-batch fermentation of Saccharomyces cerevisiae. Picque et al. [77] also used a ZnSe ATR cell for monitoring fermentations and found that whereas NIR spectra obtained from alcoholic or lactic fermentation samples contained no peaks or zones whose absorbance varied significantly, both transmission and ATR MIR could be used successfully to measure products. Fayolle et al. [78] have employed MIR for online analysis of substrate, major metabolites and lactic acid bacteria in a fermentation process (using a germanium window flow-through cell), and... 

Near infrared (NIR) spectroscopy has proved to be one of the most efficient and advanced tools for monitoring and controlling of process and product quality in food industry. A lot of work has been done in this area. This review focuses on the use of NIR spectroscopy for the analysis of foods such as meat, fruit, grain, dairy products, oil, honey, wine and other areas, and looks at the literature published in the last 10 years. 

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