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To cite this article: Ian C. Kemp , B. Christran Fyhr , Stephane Laurent , Michel A. Roques , Carda E. Groenewold ,
Evangelos Tsotsas , Alberto A. Sereno , Cathenne B. Bonazzi , Jean-Jacques Bimbenet & Mathhues Kind (2001): METHODS
FOR PROCESSING EXPERIMENTAL DRYING KINETICS DATA, Drying Technology: An International Journal, 19:1, 15-34
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DRYING TECHNOLOGY, 19(1), 15–34 (2001)
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1
SPS (Separation Processes Service), AEA Technology,
404 Harwell, Didcot, U.K.
2
University of Pau, France
3
University of Magdeburg, Germany
4
University of Porto, Portugal
5
ENSIA, Massy, France
6
University of Karlsruhe, Germany
ABSTRACT
∗
Corresponding author. E-mail: ian.kemp@hyprotech.com
15
Copyright
C 2001 by Marcel Dekker, Inc. www.dekker.com
ORDER REPRINTS
16 KEMP ET AL.
methods.
INTRODUCTION
18 KEMP ET AL.
test may thus be more representative for particles experiencing a higher relative
velocity in an industrial dryer, e.g., particles above 1 mm diameter in pneumatic
conveying and cascading rotary dryers. Conversely, the single particle test might
seem more appropriate for small particles at low relative velocity. Unfortunately,
particles this small are very difficult to suspend effectively in an airstream and this
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problem is not yet fully resolved. If a fundamental single particle drying kinetics
curve can be obtained, it can now be scaled up effectively to fluidised bed kinetics
curves (3–5). Small particles can be studied in fluidised bed or deep layer tests,
but these give markedly different drying kinetics curves to single particles due to
layer effects, even when the drying is falling-rate (6). The effect is less marked for
large particles, e.g., food; drying is mainly falling-rate, and the number of transfer
units (NTU) is small.
1. Form of the data. The major distinction is whether the raw data is in the
form of moisture content data (e.g., from continuous weighing rigs or
direct moisture measurement) or humidity data (e.g., from infra-red gas
analyzers). The former is more common.
2. Quality and quantity of the data. There may be very few points (e.g., from
periodic sampling methods), or a large number (hundreds or thousands)
from a computer data logging system. Likewise, the data may be fairly
smooth or include significant random scatter.
3. Methods used to process the data. Questions include the type of curve
or equation to fit to the data and whether to do smoothing before or after
curve fitting.
Figure 1. Drying rate and temperature curves for a particle in a crossflow dryer.
20 KEMP ET AL.
time plot. Even if the moisture curve is fairly smooth, the rate curve obtained by
differentiation will usually have a significant amount of random noise (see the
experimental plots later in this paper). It is often desirable to smooth the data to
make the rate curve less jagged. If the original moisture–time plot is not smooth
(because it consists of a small number of samples), it will be essential to perform
some sort of smoothing in order to obtain any meaningful rate curve at all.
The signal-to-noise ratio becomes worse towards the tail of the drying curve
(low moisture content and drying rate, long drying times) and, in the Krischer
curve in particular, the data points at low rate and low moisture content are very
close together. This makes it dangerous to back-calculate estimated drying times
from this part of the curve, as it involves dividing by a small number (i.e., the
drying rate) and the possible absolute error is large. For example, Fyhr and Kemp
(9) used a simple power-law characteristic drying curve to approximate a complex
rate-moisture curve obtained from an advanced model, and then back-calculated
the moisture–time curve. The results are shown in Figure 2. Over most of the
range, the approximation is indistinguishable from the original curve; if a drying
time were read from either curve, the values would be within 2% of each other.
However, at the bottom end, the curves diverge sharply; the time to dry to X = 0.02
would be read as 110 s from the characteristic curve but is 200 s in reality, which
would lead to a seriously undersized dryer. The error becomes even worse at lower
moisture contents. This is not because the characteristic curve model is faulty, but
because the fit to the data at the bottom end was poor. If the data below φ = 0.1
were refitted with a further power law curve, the CDC result would again become
very close to the results from the advanced model.
PROCESSING OF WEIGHT-LOSS
AND MOISTURE–TIME DATA
a. Use the raw data directly. This is helpful if one has only a few data
points, e.g., after an oven test with limited and infrequent sampling so
that there are only 5 to 10 data points. This method can also be used if an
accurate weighing method has been used on a reasonably sized sample
or over a very long period of time, so that there is little or no random
scatter.
b. Use the raw data, but remove outlying points, which are likely to be
spurious.
c. Use the raw data, remove outliers, and also any points whose moisture
content is greater than for the previous point. This is needed to eliminate
possible multiple solutions in computer algorithms looking for a drying
time for a given moisture content.
d. Use a simple averaging method over a number of adjacent points to
produce a piecewise curve.
e. Use the averaging method, produce the piecewise curve, and then refine
by removing any outlying points which lie too far from the curve.
f. Smooth the curve using a cubic spline fit over a number of adjacent
data points. A number of alternative spline fits may be tried, based on
different numbers of points. The best fit is most easily found by taking
the differential (gradient) of the curve, as discontinuities in the gradient
show up much more clearly than poor fits on the moisture-content points.
This also guarantees that the derived rate-time curve will be smooth.
g. Smooth the curve using a second degree polynomial on successive points
(five is a typical value). This is similar to the above method but with
a different curve form; adjusted values for moisture content X of the
median point and derivative dX/dt are computed for each experimental
point (special treatment is used for the first and last points).
h. Fit the curve to an equation of a likely theoretical form. For example,
a linear fall followed by a falling exponential, or a double exponential
(product of two exponentials), has been used, but with only limited
success (this form of equation implicitly assumes a first-order falling
rate period). A further section is needed at the start for the induction
period.
i. Use a conventional curve-fitting program to fit a variety of possible
curves to the drying curve and choose the best-fit shape. This will often
be a polynomial or rational fraction. Data may be smoothed first using
ORDER REPRINTS
22 KEMP ET AL.
24 KEMP ET AL.
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The following example, illustrating the difference between the results ob-
tained by handling the same data by different smoothing techniques, was developed
by the University of Pau. Figure 8 shows a drying curve obtained by a continuous
weighing technique. The moisture–time curve appears smooth.
However, on differentiating the curve to give the rate-time plot and the
Krischer rate–moisture plot (Fig. 9), it is clear that there is some scatter on the
ORDER REPRINTS
Figure 7. Drying curve for paddy rice smoothed by second order polynomial.
26 KEMP ET AL.
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data. There are significant random variations near the moisture peak and the bottom
part of the curve shows a good deal of noise. The latter problem occurs because the
very low drying rates involved give small changes in recorded weight and moisture
content, which are of the same order of magnitude as the noise from vibration of
the weighing device. Hence, some smoothing is desirable.
The data has been processed in two ways in Figure 10. The first is to draw
a line through all the points with a small degree of smoothing by averaging be-
tween successive points, also removing any clearly spurious outlying points. This
removes the worst of the noise at the bottom end of the Krischer plot. However, there
are still substantial variations elsewhere; the line could not be described as smooth.
The second method is to fit the line to a suitable equation. In this case, an
eighth-order polynomial has been used. This smoothes out both the lower end of
the curve and the substantial peaks and troughs at the top end. The question arises,
however, whether these peaks and troughs are due to experimental error or are
a genuine phenomenon (e.g., due to shrinkage or a change in internal moisture
movement mechanism). If the latter is the case, use of the smoothed curve will
conceal valuable information.
A third method which could be tried is to make use of drying theory and
to plot the section between X = 2.5 and X = 3.3 as a horizontal line (a constant
rate period), then fitting one or more polynomials to the remainder of the curve
(falling rate period). In this case, it is very difficult to fit a curve effectively to the
sharp dip around X = 2.2. Figure 11 shows the effect of fitting a simple straight
line for the falling rate period (first-order kinetics or drying coefficient analysis)
ORDER REPRINTS
Figure 10. Rate data smoothed by piecewise approximation and polynomial fit.
Figure 11. Rate data fitted as constant rate and falling rate sections.
ORDER REPRINTS
28 KEMP ET AL.
b
X̄ (t) = a + 2
t −c 1 t −c 2
1+e exp (1 − e)
d 2 d
Figure 12 below shows the data fitted to this equation by a least-squares method.
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Clearly a smooth curve has been obtained. However, comparison with the origi-
nal data above shows that the curve is markedly different from the original data
and presents a completely misleading impression of the results of the original
experiment; important information has been concealed.
An important point from all these items taken together is that, if smoothing is
applied, the raw data should always be retained in parallel, to use as a cross-check
and to ensure that the smoothing has not distorted some important aspect.
For practical dryer design, a common method would be to transform these
curves back to the moisture–time form, then find the times from the curve corre-
sponding to the inlet and outlet moisture contents. The required drying time would
be the difference between these. Figure 2 showed the effects of inaccuracies in fit-
ting the Krischer curve on the back-calculated drying curve. Small differences have
little effect, except at extremely low drying rates and moisture contents. On this
basis, if the curves above were transformed back to drying curves, the smoothed
curve, the eighth-order polynomial and the characteristic curve (after an initial con-
stant rate period) would give excellent fits to the raw data and an estimate of drying
time well within 5%, which would give an accurate dryer design. Using first-order
kinetics would give a reasonable fit, whereas fitting to the equation would give a
very poor fit and a major error in estimated size of the resulting dryer, especially
in the early stages of drying at high moisture contents.
In summary, some smoothing may be useful to eliminate the noise and
random variation in the drying curve, but the raw data should always be re-
tained for comparison. Obviously erroneous outlying points should be removed
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Plots of humidity against time are obtained from experimental apparatus such
as the SPS drying kinetics rig (11,12), which measure the outlet humidity rather
than weight loss. An infra-red gas analyser (IRGA) may be used to give a large
number of humidity recordings at intervals of 5 s or less. A mass balance converts
this directly to the plot of drying rate against time, and this can be integrated to
give the moisture–time plot. It is essential to cross-check the calculated moisture
content reduction with experimental values of inlet and outlet moisture content
obtained by oven tests.
The humidity signal often has some scatter on it, and smoothing will be
necessary to give a smooth drying rate vs. time curve. Figure 13 shows a typical
plot and Figure 14 shows smoothed and unsmoothed drying rate curves. A Fast
Fourier transform has been used for the smoothing. Note, however, that when the
data is integrated to form the moisture–time graph in Figure 15, it appears perfectly
smooth, whether the rate data is in raw or smoothed form.
The recommended method for dealing with a humidity–time curve is as
follows.
ORDER REPRINTS
30 KEMP ET AL.
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r Smooth the raw humidity–time data (which usually has a lot of random
scatter) using a Fast Fourier transform. A separate smoothing is desirable
for the induction period, as otherwise the humidity peak tends to be
artificially lowered.
r Convert the humidity–time data to drying rate–time data based on recor-
ded gas velocity and mass of solids present.
Figure 14. Drying rate data from mass balance, smoothed and unsmoothed.
ORDER REPRINTS
Note that small errors in the inlet humidity can lead to big final errors in the final
drying curve, as the drying rate is proportional to the difference between inlet and
outlet humidity. Ideally, the inlet humidity will be precisely the same throughout
the experiment, but in practice fluctuations or drift may occur. At the tail end,
where the difference is small, an incorrect inlet humidity value will lead to a finite
32 KEMP ET AL.
inlet humidity.
This is a huge subject in itself and would require a further paper to cover
adequately. Some simple points can be made, however.
r The existence, or otherwise, of a constant rate drying period will indicate
whether the material goes through a heat-transfer-controlled phase, or is
limited by internal moisture transport throughout (the latter being more
common at high drying intensities).
r The smoothness of the data obviously gives an indication of the quality
of the original experiments.
r Many materials fit reasonably well to a simple first-order kinetics curve
(linear fall on the Krischer plot), especially in the final stages of drying.
The intercept on the moisture content axis indicates whether there is a
significant equilibrium moisture content.
r There is rarely, if ever, a sharp transition from constant rate drying (ex-
ternal heat and mass transfer control) to falling rate drying (internal mass
transfer control). Normally, the critical moisture content has to be ob-
tained by projection of fitted lines for the two periods to a meeting point
which lies slightly above the experimental curve.
r It is important to remember that nearly all drying curves are distorted
from their theoretical form by layer effects, because there are finite NTUs
in the experiments. This again tends to give gentle curves and smooth
transitions rather than sharply defined horizontal and sloping sections.
In particular, it may give an apparent constant rate period that is actually
due to saturation of the air passing through the bed; the material itself is
in falling-rate hindered drying.
CONCLUSIONS
measure and need to be adjusted to allow for the geometry of the actual
drying system to be used. For all methods, scale-up and scale-down may
be required to allow for differences such as bed depth between the ex-
periment and the full-scale dryer. Saturation in thick layers must always
be checked for.
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ACKNOWLEDGMENTS
This work was carried out under the QUID (Quality in Drying) project funded
by the CEC under the ‘Training and Mobility of Researchers’ scheme. The project
is coordinated by the University of Lund; other participants are the Universities
of Eindhoven, Karlsruhe, Magdeburg, Pau and Porto, ENSIA-Massy, and AEA
Technology plc.
ORDER REPRINTS
34 KEMP ET AL.
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