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CHIPS
Blow Tank
Washers
PULP
InfraSpec NR800
Causticizers
Evaporators
Lime Kiln
Slaker
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Measurement of Alkali The spectra of white liquor a nd green liquor are shown in Fig.3. Changes in the absorbance spectra are related to changes in the hydrogen bonding of water caused by the concentration of the various alkali salts dissolved in the water. PLS calibration models were created for NaOH, Na2S and Na2CO3 concentrations and are shown in Figures 4-6. Correlations for all 3 calibrations are 0.97 or greater and the Standard Error of the Prediction (SEP) is approximately 1 g/L for all 3 calibrations. A key point to be noted is that these spectra and calibrations were made at a fixed temperature. One issue that must be addressed in this application of FTNIR is the change in the spectrum of water caused by temperature. Figure 7 shows the spectrum of water at various temperatures. The change in the spectrum due to temperature change is great compared to the change in spectrum caused by the alkali concentration.
Figure 4: Predicted vs. Measured Plot for NaOH (g/L)
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There are basically three ways to deal with the effects of temperature on the spectra such that it does not affect the measurement. The first, and most obvious is to control the sample temperature using a sample conditioning system. Figure 8 shows such a system for white liquor, green liquor and black liquor. Note the provisions for flushing the system with water and with Hydrochloric Acid to remove deposits. This approach has the advantage of being the most precise, but is also usually the most expensive.
80 o C
30 o C
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Another approach is to create the calibration at a constant and convenient temperature, then to measure the effect of temperature on the output of the calibration model. Temperature changes in the sample often apply a linear bias to the output that can be compensated by a temperature measurement and a factor applied to the analyzer output.
Temperature Probe
The third approach is to include the variations in temperature into the calibration model. One of the advantages of Partial Least Squares (PLS) calibration models is that they separate effects that are not correlated with the measurement. To do this, the set of samples used to make the calibration model (typically 30-50 samples) must have spectra taken over the entire range of temperatures likely to be seen. This need not be done systematically, that is, by varying the temperature of each sample by set amounts. The spectral scans can be taken at random temperatures, provided the range of temperatures covers the range likely to be observed in the process. This approach is referred to as making the model robust to temperature effects.
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Figure 11 shows an on-line trend graph of FT-NIR measurements on green liquor. Figure 12 shows the measurement of effective alkali in black liquor.
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Other Applications of FT-NIR in Pulp and Paper Processes Measurements of kappa number in black liquor have been reported i. Near infrared spectral measurements have been used to predict pulp yield ii. In-situ ATR probes have been used on spent liquors iii. Andersson and Wilsoniv report excellent measurements of effective alkali (EA), lignin, Xylan, total organic material, Cellulose and Glucomannan among other parameters in black liquor by NIR. Clearly, we have only begun to scratch the surface of applications for NIR in the pulp and paper industry. Given the capital-intensive nature of the industry, and the size of the facilities, the economic justifications will be found for new and creative applications of NIR technology over the next several years.
i
R. E. Hodges, Applications of near infrared spectroscopy in the pulp and paper industry, PhD thesis, Auburn University, Auburn Alabama, US, 1997. ii T. Lindgren and U. Edlun, Prediction of lignin content and pulp yield, Nor. Pulp Pap. Res. J., 13(1):78-80, 1998. iii V.M. Saucedo and G.A. Krishnagopalan, Applications of in-situ near-infrared analysis for the measurement of cooking liquor components during kraft pulping, J. pulp Paper Sci., 26(1):25-30, 2000. iv N. Andersson and D. I. Wilson, http://www.ee.kau.se/forskning/ModSim/nir_tappi.pdf
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