Fiber measurements, calibration

Inject the SPME fiber being calibrated through the septum and measure peak area (see Basic Protocol), but expose the fiber to the headspace for exactly 5 min. 

Lischer DJ, Louge M. Optical fiber measurements of particle concentration in dense suspensions calibration and simulation. Applied Optics 31 5106-5113, 1992. 

Bauer et al. describe the use of a noncontact probe coupled by fiber optics to an FT-Raman system to measure the percentage of dry extractibles and styrene monomer in a styrene/butadiene latex emulsion polymerization reaction using PLS models [201]. Elizalde et al. have examined the use of Raman spectroscopy to monitor the emulsion polymerization of n-butyl acrylate with methyl methacrylate under starved, or low monomer [202], and with high soUds-content [203] conditions. In both cases, models could be built to predict multiple properties, including solids content, residual monomer, and cumulative copolymer composition. Another study compared reaction calorimetry and Raman spectroscopy for monitoring n-butyl acrylate/methyl methacrylate and for vinyl acetate/butyl acrylate, under conditions of normal and instantaneous conversion [204], Both techniques performed well for normal conversion conditions and for overall conversion estimate, but Raman spectroscopy was better at estimating free monomer concentration and instantaneous conversion rate. However, the authors also point out that in certain situations, alternative techniques such as calorimetry can be cheaper, faster, and often easier to maintain accurate models for than Raman spectroscopy, hi a subsequent article, Elizalde et al. found that updating calibration models after... 

Sampling mode effects The goal was to be able to measure at-line, with no sample preparation at all, using a fiber-optic probe or a remote sampling head. However, the area sampled by the hber-optic probe is much smaller than for the sample transport module. It was found that the remote (probe) spectra were very similar to the static (sample transport) spectra, but the baselines were shifted significantly higher and the absorbance peaks consequently reduced in intensity as before, the characteristic peak positions were not affected. Calibration models developed using spectra obtained with the hber-optic probe performed equivalently to those developed with the sample transport module. 

Suppose the pan of a balance is positioned at some convenient location below the surface of a dispersion. As sedimentation occurs, the settled material collects on the balance pan. The total weight W of the material on the pan is measured at various times t, either by adding counterweights to a second pan or by noting the displacement of a calibrated fiber that supports the pan. The following example suggests how this kind of data is analyzed. 

Here is a student procedure to measure nicotine in urine. A 1.00-mL sample of biological fluid was placed in a 12-mL vial containing 0.7 g Na2CO , powder. After 5.00 pig of the internal standard 5-aminoquinoline were injected, the vial was capped with a Teflon-coated silicone rubber septum. The vial was heated to 80°C for 20 min and then a solid-phase microextraction needle was passed through the septum and left in the headspace for 5.00 min. The fiber was retracted and inserted into a gas chromatograph. Volatile substances were desorbed from the fiber at 250°C for 9.5 min in the injection port while the column was at 60°C. The column temperature was then raised to 260°C at 25°C/min and eluate was monitored by electron ionization mass spectrometry with selected ion monitoring at m/z 84 for nicotine and m/z 144 for internal standard. Calibration data from replicate... 

Optical devices have also been used as transducers. Laser fiber-optics allows high intensity light to travel a long distance using fibrous size carrier. The stable and intense light beam not only provides calibration stability but also makes all the detecting techniques faster and more sensitive. In addition to the UV-VIS absorbance and fluorescence intensity, measurements of multiple reflections, surface plasmon resonance, and total internal reflection fluorescence had recently been used (12, 13, 14). 

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