Mid-IR analysis

FT-IR has been used for both characterization [111] and quantitation [112,113] of residual lignin in chemical pulps. Due to the low lignin concentration, the infrared band at 1510 cm- is most suited for the latter purpose. Good correlations between kappa number and IR intensity were found for kraft pulps produced from a range of hardwoods and softwoods. The advantage of mid-IR analysis was that no sample preparation was required. 

Mid-IR analysis has been used in the textile industry for the past few years in some specific applications that are worth mentioning along with the near-IR applications. Some background information on related textile products and processes will be provided to establish the need for these measurements. 

Infrared spectroscopy (mid-IR range) has been used extensively in characterizing textile materials for both qualitative and quantitative analyses. These tests include detection of contaminants, amount of lubricants on yarn and fabrics, and information relating to the polymer structure and morphology. In this section, the use of mid-IR analysis to obtain useful infor-... 

Radiometry. Radiometry is the measurement of radiant electromagnetic energy (17,18,134), considered herein to be the direct detection and spectroscopic analysis of ambient thermal emission, as distinguished from techniques in which the sample is actively probed. At any temperature above absolute zero, some molecules are in thermally populated excited levels, and transitions from these to the ground state radiate energy at characteristic frequencies. Erom Wien s displacement law, T = 2898 //m-K, the emission maximum at 300 K is near 10 fim in the mid-ir. This radiation occurs at just the energies of molecular rovibrational transitions, so thermal emission carries much the same information as an ir absorption spectmm. Detection of the emissions of remote thermal sources is the ultimate passive and noninvasive technique, requiring not even an optical probe of the sampled volume. 

FTIR instrumentation is mature. A typical routine mid-IR spectrometer has KBr optics, best resolution of around 1cm-1, and a room temperature DTGS detector. Noise levels below 0.1 % T peak-to-peak can be achieved in a few seconds. The sample compartment will accommodate a variety of sampling accessories such as those for ATR (attenuated total reflection) and diffuse reflection. At present, IR spectra can be obtained with fast and very fast FTIR interferometers with microscopes, in reflection and microreflection, in diffusion, at very low or very high temperatures, in dilute solutions, etc. Hyphenated IR techniques such as PyFTIR, TG-FTIR, GC-FTIR, HPLC-FTIR and SEC-FTIR (Chapter 7) can simplify many problems and streamline the selection process by doing multiple analyses with one sampling. Solvent absorbance limits flow-through IR spectroscopy cells so as to make them impractical for polymer analysis. Advanced FTIR... 

Both a pneumatic heated nozzle system [487] and an ultrasonic nozzle/vacuum system [699] have been described for removing the troublesome solvent in order to simplify IR analysis. The former system (LC Transform ) has been commercialised [700], and allows full use of the mid-IR spectral range by providing analyte films free from solvent interference. The evaporative... 

TGA, iodometric, mid-IR, luminescence (fluorescence and phosphorescence) and colour formation (yellowness index according to standard method ASTM 1925) were all employed in a study of aspects of the thermal degradation of EVA copolymers [67], Figure 23 compares a set of spectra from the luminescence analysis reported in this work. In the initial spectra (Figure 23(a)) of the EVA copolymer, two excitation maxima at 237 and 283 nm are observed, which both give rise to one emission spectrum with a maximum at 366 nm weak shoulders... 

Similar to IR sensors, process analysis is the prevalent application area. Due to the applicability of standard VIS instrumentation, Raman probes have been used for more than two decades65, 66. Typically, Raman probes are applied where near-IR probes fail and hence are in direct competition to mid-IR probes. 

In each of the aforementioned studies, qualitative IR spectroscopy was used. It is important to realize that IR is also quantitative in nature, and several quantitative IR assays for polymorphism have appeared in the literature. Sulfamethoxazole [35] exists in at least two polymorphic forms, which have been fully characterized. Distinctly different diffuse reflectance mid-IR spectra exist, permitting quantitation of one form within the other. When working with the diffuse reflectance IR technique, two critical factors must be kept in mind when developing a quantitative assay (1) the production of homogeneous calibration and validation samples, and (2) consistent particle size for all components, including subsequent samples for analysis. During the assay development for... 

The cost per analysis point and the projected payback are only two metrics used to evaluate the feasibility of installing a process analyzer. If a spectrometer replaces an existing service intensive analyzer then that is a positive situation. Also, because of the flexibility of infrared analyses, it is feasible that a mid-IR analyzer might replace several existing analyzers it is a case where direct chemical information from IR can be more important than certain inferential methods that only provide indirect information. Also, if the only other... 

Diffuse reflectance is an excellent sampling tool for powdered or crystalline materials in the mid-IR and near-IR spectral ranges. Heated reaction chambers for diffuse reflectance allow the study of catalysis and oxidation reactions in situ, and can evaluate the effects of temperature and catalyst behavior. Scratching sample surfaces with abrasive paper and then measuring the spectra of the particles adhering to the paper allows for analysis of intractable solids. Perhaps one of the greatest additional benefits is that this system is amenable to automation. 

UV-Vis linear dichroism and (mid-)IR ATR IR analysis have been used to explain the possible association between DNA and the flavonols quercetin, rutin (quercetin-3-rutino-side), and morin (3,5,7,2, 4 -pentahydroxyflavone) in solution.These nucleophilic flavonoids were shown to bind DNA by intercalation with an interaction having similar nature and geometry however, under comparable conditions, quercetin exhibited a greater number... 

Modern infrared (IR) spectroscopy is a versatile tool applied to the qualitative and quantitative determination of molecular species of all types. Its applications fall into three categories based on the spectral regions considered. Mid-IR (MIR) is by far the most widely used, with absorption, reflection, and emission spectra being employed for both qualitative and quantitative analysis. The NIR region is particularly used for routine quantitative determinations in complex samples, which is of interest in agriculture, food and feed, and, more recently, pharmaceutical industries. Determinations are usually based on diffuse reflectance measurements of untreated solid or liquid samples or, in some cases, on transmittance studies. Far-IR (FIR) is used primarily for absorption measurements of inorganic and metal-organic samples. 

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