You are on page 1of 23

See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/244603042

Methods for processing experimental drying kinetics data

Article  in  Drying Technology · January 2001


DOI: 10.1081/DRT-100001350

CITATIONS READS

94 1,571

10 authors, including:

Ian C. Kemp Michel André Roques


GlaxoSmithKline Université de Pau et des Pays de l'Adour
70 PUBLICATIONS   1,420 CITATIONS    45 PUBLICATIONS   919 CITATIONS   

SEE PROFILE SEE PROFILE

Evangelos Tsotsas Alberto M. Sereno


Otto-von-Guericke-Universität Magdeburg University of Porto
480 PUBLICATIONS   4,137 CITATIONS    68 PUBLICATIONS   2,322 CITATIONS   

SEE PROFILE SEE PROFILE

Some of the authors of this publication are also working on these related projects:

Dynamics of fluidised bed layering granulation View project

Simulation of the drying process of functional oil microcapsulation by spray dryer View project

All content following this page was uploaded by Alberto M. Sereno on 18 July 2015.

The user has requested enhancement of the downloaded file.


This article was downloaded by: [b-on: Biblioteca do conhecimento online UP]
On: 17 June 2013, At: 09:27
Publisher: Taylor & Francis
Informa Ltd Registered in England and Wales Registered Number: 1072954 Registered office: Mortimer
House, 37-41 Mortimer Street, London W1T 3JH, UK

Drying Technology: An International Journal


Publication details, including instructions for authors and subscription information:
http://www.tandfonline.com/loi/ldrt20

METHODS FOR PROCESSING EXPERIMENTAL DRYING


KINETICS DATA
a a b b
Ian C. Kemp , B. Christran Fyhr , Stephane Laurent , Michel A. Roques , Carda E.
c d e f
Groenewold , Evangelos Tsotsas , Alberto A. Sereno , Cathenne B. Bonazzi , Jean-
f g
Jacques Bimbenet & Mathhues Kind
a
AEA Technology, SPS (Separation Processes Service), 404 Harwell, Didcot, U.K.
b
University of Pau, France
c
University of Magdebg, Germany
d
University of Magdeburg, Germany
e
University of Porto, Portugal
f
ENSIA, Massy, France
g
University of Karlsruhe, Germany
Published online: 06 Feb 2007.

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

To link to this article: http://dx.doi.org/10.1081/DRT-100001350

PLEASE SCROLL DOWN FOR ARTICLE

Full terms and conditions of use: http://www.tandfonline.com/page/terms-and-conditions

This article may be used for research, teaching, and private study purposes. Any substantial or systematic
reproduction, redistribution, reselling, loan, sub-licensing, systematic supply, or distribution in any form to
anyone is expressly forbidden.

The publisher does not give any warranty express or implied or make any representation that the contents
will be complete or accurate or up to date. The accuracy of any instructions, formulae, and drug doses
should be independently verified with primary sources. The publisher shall not be liable for any loss, actions,
claims, proceedings, demand, or costs or damages whatsoever or howsoever caused arising directly or
indirectly in connection with or arising out of the use of this material.
DRYING TECHNOLOGY, 19(1), 15–34 (2001)
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

METHODS FOR PROCESSING


EXPERIMENTAL DRYING KINETICS DATA

Ian C. Kemp,1,∗ B. Christran Fyhr,1 Stephane Laurent,2


Michel A. Roques,2 Carda E. Groenewold,3 Evangelos
Tsotsas,3 Alberto A. Sereno,4 Cathenne B. Bonazzi,5
Jean-Jacques Bimbenet,5 and Mathhues Kind6

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

This paper provides a review of methods for processing the


data obtained from drying kinetics rigs and pilot-plant trials. Differ-
ent methods for fitting and smoothing drying curves are compared,
aiming to generate curves that are usable in industrial design with-
out losing vital information by oversmoothing. Generally, plots of
drying rate need more smoothing than moisture content data. Spe-
cial care is needed at low drying rates and moisture contents. It is
shown that some popular methods of processing data, including use
of smoothing programs or fitting to equations, may generate drying
curves which are seriously in error. Recommendations are made for
reliable methods of processing data; cubic splines have been found


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.

to be effective for moisture–time curves. It is important to retain


the original raw experimental data as a cross-check, as smoothing
can conceal valuable information.

Key Words: Drying curve; Rate data; Smoothing; Recommended


Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

methods.

INTRODUCTION

Numerous articles have appeared describing experimental apparatus to


record drying kinetics and even more numerous papers that present results from
such experiments. However, the mundane but important subject of how to process
the experimental data in the most reliable way has received relatively little attention.
The data obtained from drying kinetics experiments typically contains inac-
curacies, spurious points, and noise. It is important to remove these and obtain a
smoothed curve that can be used for design purposes. However, important infor-
mation must not be concealed. In particular, oversmoothing or using the wrong
method may conceal or distort information, which may lead to substantial errors
in the design of a full-scale dryer.
The Council of the European Communitities (CEC) has funded eight
European research laboratories to work together in drying in the QUID (Quality in
Drying) project. Participants are the Universities of Lund, Eindhoven, Karlsruhe,
Magdeburg, Pau, Porto, and ENSIA-Massy, and AEA Technology plc. In the course
of this work, it was necessary to understand the different methods used for pro-
cessing the data. The methods used for one type of drying experiment may be
inappropriate for another. Nevertheless, a reasonable consensus was reached and
is presented here. It is hoped that this will be of use to drying researchers world-
wide in giving a unified approach to the reporting of data. In particular, it is hoped
that this will present an easy guide to best practice for researchers who are new to
the field of drying.

METHODS OF OBTAINING DRYING KINETICS DATA

There are three principal methods of obtaining drying kinetics data:


1. Periodic sampling or weighing. A sample may be extracted at intervals
and its moisture content determined by laboratory methods, or the entire
sample of material may be weighed and then reintroduced into the drying
apparatus. These methods are slow and tend to give very few points on
a moisture–time graph.
2. Continuous weighing. A sample is mounted on a microbalance, or an
accurate balance suspended in a drying tunnel, and its weight is recorded
ORDER REPRINTS

PROCESSING DRYING KINETICS DATA 17

continuously. This gives a much larger number of points on the


moisture–time graph. However, the small changes in weight involved
can be concealed by random noise, e.g., due to vibration of the sample
in the airstream.
3. Intermittent weighing. The sample is mounted on a balance in an air
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

stream as above, and, at intervals, the airflow is cut off or diverted, so


that an accurate weight reading can be obtained when the system has
stabilised (which takes a few seconds). It has been found that this does
not affect the kinetics unless drying times are very short (a few minutes).
4. Indirect methods. The rate of water vapour evolution can be measured,
e.g., by measuring the air humidity emerging from the sample chamber,
using an infrared gas analyser or simular apparatus. The rate of moisture
loss is then back-calculated.
The best choice from these approaches will depend on many factors; particle
size, initial and final moisture content, predominant drying regime (unhindered or
falling-rate), air velocity, level of accuracy required for the data, and availability
of measurement equipment.
The configuration of the drying apparatus is also important. Tests can be
done on single particles on a microbalance or in a drying tunnel, or on thin layers,
medium or deep beds, the latter using cross-circulation, through-circulation, flu-
idisation or conduction heating. In general, on a larger scale, the signal is stronger
(bigger weight change or higher outlet humidity), but information is concealed
because the data is the average from a large number of particles rather than a few.
For beds and thick layers, it is difficult or impossible to ensure that all the parti-
cles have the same temperature and exposure history. Even for thin layers, some
scaledown is necessary to obtain a fundamental drying kinetics curve, and this is
difficult to do reliably (1).
The recording method and the size of the sample affect the method to be
used. For fundamental single-particle kinetics, as recorded in the Magdeburg
drying tunnel, the signal-to-noise ratio is weaker and the moisture–time curve
shows considerable random scatter. For bulk drying experiments and slow drying
materials, the weighing can be more accurate and is less susceptible to vibra-
tion, so the initial curve can be quite smooth. However, less information is ob-
tained on the fundamental kinetics because of the higher number of transfer units
(NTUs).
During recent work in the QUID project, results from single and multiple
particle tests in the University of Magdeburg drying tunnel have been compared
with thin-layer tests at SPS at Harwell (2). The drying curves obtained were broadly
similar but the critical moisture content was higher for the thin-layer tests because
the rig uses a higher velocity. (Low velocities make layer effects worse in a thin-
layer test, as the number of transfer units increases. Conversely, high velocities
gave too much vibration and signal noise in the drying tunnel.) The thin-layer
ORDER REPRINTS

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
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

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.

TYPES OF DATA TO BE PROCESSED

There are several important points to consider initially:

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.

There are a number of useful curves that are interrelated:

a. Drying curve—moisture content vs. time. (X vs. t). Obtained directly


from weight loss-time data. Integral of (b).
b. Drying rate curve—drying rate vs. time. (−dX/dt vs. t, or N vs. t).
Obtained directly from humidity–time data. Differential of (a). It tends
to be much more jagged than the moisture content curve, with lots of
random variation.
c. Time-independent or Krischer curve—drying rate vs. moisture content.
(−dX/dt vs. X , or N vs. X ). Usually derived from the combination of
(a) and (b). This curve is used as the basis for the characteristic curve
scaling method.
ORDER REPRINTS

PROCESSING DRYING KINETICS DATA 19


Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

Figure 1. Drying rate and temperature curves for a particle in a crossflow dryer.

d. Temperature-time plot—shows how the sample temperature varies dur-


ing the experiment.
Figure 1 shows the four interrelated curves obtained by simulation of a single
particle undergoing convective drying in a hot air stream at a constant 150◦ C.
Under the chosen conditions, this material is assumed to show an induction (initial
heating) stage, an unhindered drying (constant rate) period, and a hindered drying
(falling rate) period.
It is useful and, indeed, common, to interconvert between the three different
types of drying curve. For example, a set of moisture–time data (a) may be recorded
in an experiment. This batch drying curve is then differentiated to give the drying
rate-time curve (b), and the Krischer rate–moisture curve (c) is then produced by
combining the other two curves. A characteristic curve (7,8) can then be fitted to
the data from the Krischer curve. If it is now desired to design a dryer at different
inlet conditions, the new maximum drying rate is calculated from external heat and
ORDER REPRINTS

20 KEMP ET AL.

mass transfer considerations, and a new Krischer curve is produced by scaling up


the batch drying curve. By taking the inverse of the drying rate, a moisture–time
curve for the new conditions can be generated, and the required time to dry from the
initial moisture content to the desired final moisture can be read off from the graph.
In general, it is found that the moisture–time plot is smoother than the rate-
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

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.

Figure 2. Effect of an approximate data fit on rate-moisture and moisture–time curves.


ORDER REPRINTS

PROCESSING DRYING KINETICS DATA 21

PROCESSING OF WEIGHT-LOSS
AND MOISTURE–TIME DATA

Possible methods for dealing with a moisture–time curve include the


following:
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

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.

programs such as TableCurve and MS-Excel’s Trendline function. There


will be no real theoretical basis for such a fit; it is simply a correlation.
j. Develop a drying model for the particular material (which may include
allowances for NTUs, etc.), and fit the data to adjustable parameters in
the model. This is particularly effective for families of materials that can
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

be expected to fit a given model, e.g., various foods.


The drying rate-time and rate-moisture curves must now be derived from the
moisture–time curve. This is usually done by numerical differentiation e.g., by
a finite-difference method. The rate curves are often much more jagged than the
moisture–time curve, and it may be useful to resmooth to give an acceptable-
looking curve.
Figure 3 shows a drying curve for silica gel, obtained using a thin-layer
kinetics test. It has been successfully smoothed using a cubic spline. The derivative
of the curve has also been calculated, and this indicates the shape of the drying rate
curve. There is some noise, especially at the lower end, but the curve is smooth and
the fit is good. In contrast, Figure 4 shows a curve that has been undersmoothed
(the rate curve is still jagged) and one that has been oversmoothed (the rate curve
is very smooth, but the fit to the original moisture content curve is now poor). In
practice, it is often best to smooth the rate–time curve separately, addressing only
the areas where there is a clear deviation (e.g., beyond about 40 s in the curves
in Figs. 3 and 4). Figure 5 illustrates the effect of attempting to fit the curve to

Figure 3. Moisture–time curve smoothed by cubic spline fit.


ORDER REPRINTS

PROCESSING DRYING KINETICS DATA 23


Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

Figure 4. Undersmoothed and oversmoothed drying curves.

equations with a falling exponential tail (corresponding to first-order kinetics).


The equations fail totally to allow for the induction period, but are also a poor fit
generally, despite their reasonable theoretical basis.
The more irregular the moisture–time curve, the more smoothing is neces-
sary before trying to calculate drying rates. Figure 6 shows data obtained from a

Figure 5. Drying curve fitted to theoretical equation forms.


ORDER REPRINTS

24 KEMP ET AL.
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

Figure 6. Smoothing of direct weighing data from drying tunnel experiment.

direct-weighing experiment of a small mass of particles in a drying tunnel. The


signal-to-noise ratio is low and there is some evidence of a regular periodic os-
cillation. However, this data has again been successfully smoothed by a spline fit.
This was helped by removing obviously erroneous outlying points from the data
before performing the final fit.
Figure 7 shows a drying curve for paddy rice, obtained from a thin layer dry-
ing experiment with periodic direct weighing of the entire sample and temporary
deviation of the drying air. It has been successfully smoothed using a sliding
polynomial, and the rate-time curve has been derived at each point from the cor-
responding polynomial. There is some noise in the rate-time curve due to the very
low drying rate, but the moisture content at each point is very close to the raw
experimental one.

Case Study on Curve Smoothing

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

PROCESSING DRYING KINETICS DATA 25


Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

Figure 7. Drying curve for paddy rice smoothed by second order polynomial.

Figure 8. Experimentally recorded moisture–time curve.


ORDER REPRINTS

26 KEMP ET AL.
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

Figure 9. Drying rate data obtained by differentiation, unsmoothed.

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

PROCESSING DRYING KINETICS DATA 27


Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

Figure 10. Rate data smoothed by piecewise approximation and polynomial fit.

and a characteristic curve (approximated in this case by two power-law sections


with smooth transitions).
An alternative method is to fit the data to an equation. The following equation
has been proposed as appropriate for this system:

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.
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

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

Figure 12. Rate data fitted to correlation equation.


ORDER REPRINTS

PROCESSING DRYING KINETICS DATA 29

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
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

before smoothing. The best general-purpose smoothing method is probably a cubic


spline or localized sliding polynomial. However, overall polynomials and constant-
rate/characteristic curve fits have also been successful. Simple first-order kinetics
may be useful if very limited test information is available. The derived drying
rate curve will fluctuate more, and it can be smoothed by methods similar to that
recommended below for humidity curves, though Hager et al. (10) recommended
retaining the raw data for the drying rate and not smoothing at all.
In general, fitting the results to an equation of predetermined form is not
recommended. However, if the drying process is definitely known to follow a
particular form of kinetics, then an equation may be used. This approach has
been used successfully by the University of Porto to process drying kinetics for
food materials. In contrast, AEA Technology in early versions of their FLUBED
fluidized bed-drying software attempted to fit drying curves with either a linear
section followed by a falling exponential, or two falling exponentials combined,
as shown in Figure 5. (This form of curve would correspond to first-order drying
kinetics). It was found that the fit was often poor, even for materials that were quite
close to first-order kinetics.

PROCESSING OF HUMIDITY–TIME DATA

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.
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

Figure 13. Experimentally recorded humidity–time plot.

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

PROCESSING DRYING KINETICS DATA 31


Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

Figure 15. Drying curve found by integration, smoothed/unsmoothed.

r Integrate the rate-time data to a moisture content-time curve and cross-


check against initial and final moisture content obtained from oven tests.
The two results should agree to within 5%. The moisture–time curve
obtained is usually very smooth if enough humidity data points were
recorded.
r Plot the rate-moisture curve; no further smoothing should be necessary.
Derive a characteristic drying curve if desired.

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

Figure 16. Krischer (rate-moisture) curve, smoothed/unsmoothed.


ORDER REPRINTS

32 KEMP ET AL.

calculated drying rate, whereas it should be tending to zero. It is often possible


to identify this situation by examining the moisture–time curve derived from the
rate data; either it continues to descend gradually with a steady gradient at the end
of drying instead of levelling off, or it reaches a minimum and then rises again.
In both cases, the curves should be recalculated using slightly different values of
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

inlet humidity.

INTERPRETATION OF THE EXPERIMENTAL DATA

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

r It is important to choose an appropriate form of drying kinetics test.


Single-particle kinetics curves are fundamental, but they are hard to
ORDER REPRINTS

PROCESSING DRYING KINETICS DATA 33

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.
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

r For processing moisture–time data obtained by a weight-loss method, the


best general-purpose method appears to be a cubic spline fit.
r Humidity-time data may be smoothed, converted to drying rate v. time
by mass balance, and integrated to give a moisture–time curve.
r Don’t discard the raw data—retain it throughout. Whatever method is
used, smoothing tends to conceal information. The raw data provides a
“sanity check” on any smoothed curve, and any related curves derived
from it.
r Dubious points should be removed or adjusted before fitting. This is
preferable to fitting to an equation or using standardized smoothing rou-
tines.
r An equation-based method should only be used if one is confident that
the system is definitely going to fit that type of model. Otherwise, the fit
can be extremely poor.
r Certain regions of curves derived from others are inherently prone to er-
ror, as they are differences of large numbers or reciprocals of small ones.
Particular care is needed when deriving time data from the low-moisture
region of the Krischer rate-moisture curve.
r Wrong results may be obtained even with the right method (e.g., cu-
bic splining), by using too strong a smoothing factor, again concealing
information.
r The human eye is often the best means of fitting the data or, at least, of
checking a computer-generated fit to make sure that it looks sensible!
r The rate data usually has more noise than the moisture-content data, and
it is often best to do an initial fit on the moisture–time curve using a cu-
bic spline, followed by smoothing the later part of the drying rate curve
separately.

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.

REFERENCES

1. Fyhr, C.; Kemp, I.C. Evaluation of the Thin-Layer Method Used for
Measuring Single Particle Drying Kinetics. Transact. IChemE, Part A, 1998,
76 (A7), 815–822.
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

2. Hirschmann, C.; Fyhr, C.; Tsotsas, E.; Kemp, I.C. Comparison of Two Ba-
sic Methods for Measuring Drying Curves: Thin Layer Method and Dry-
ing Channel, Proceedings of the 11th International Drying Symposium,
Halkidiki, Greece, 1998; Vol. A224–231. Ziti Editions, Thessalonīkī, Greece.
3. Tsotsas, E. From Single Particle to Fluid Bed Drying Kinetics. Drying Tech-
nol. 1994, 12, 1401–1426.
4. Burgschweiger, J.; Groenewold, H.; Hirschmann, C.; Tsotsas, E. From Hy-
groscopic Single Particle to Batch Fluidized Bed Drying Kinetics. Can. J.
Chem. Eng. 1999, 77, 333–341.
5. Fyhr, C.; Kemp, I.C. Mathematical Modelling of Batch and Continuous Well-
mixed Fluidised Bed Dryers. Chem. Eng. Process. 1999, 38, 11–18.
6. Fyhr, C.; Kemp, I.C.; Wimmerstedt, R. Mathematical Modelling of Fluidised
Bed Dryers with Horizontal Dispersion, Chem. Eng. Process. 1999, 38, 89–
94.
7. van Meel, D.A. Adiabatic Convection Batch Drying with Recirculation of
Air. Chem. Eng. Sci. 1958, 9, 36–44.
8. Keey, R.B. Drying of Loose and Particulate Materials; Hemisphere: New
York, 1992.
9. Fyhr, C.; Kemp, I.C. Comparison of Different Kinetics Models for Single
Particle Drying Kinetics. Drying Technol. 1998, 16 (7), 1339–1369.
10. Hager, J.; Hermansson, M.; Wimmerstedt, R. Modelling Steam Drying of a
Single Porous Ceramic Sphere—Experiments and Simulations. Chem. Eng.
Sci. 1997, 52, 1253–1264.
11. McKenzie, K.A.; Bahu, R.E. Material Model for Fluidised Bed Drying,
Drying ’91 (7th Int. Drying Symp. Prague, Czechoslovakia, Aug. 1990);
A.S. Mujumdar and I. Filková (Ed.); Elsevier: Amsterdam, 1991; 130–141.
12. Langrish, T.A.G.; Bahu, R.E.; Reay, D. Drying Kinetics of Particles from
Thin Layer Drying Experiments, Drying ’91 (7th Int. Drying Symp. Prague,
Czechoslovakia, Aug. 1990); A.S. Mujumdar and I. Filková (Ed.); Elsevier,
Amsterdam 1991; 196–206.
Request Permission or Order Reprints Instantly!

Interested in copying and sharing this article? In most cases, U.S. Copyright
Law requires that you get permission from the article’s rightsholder before
using copyrighted content.

All information and materials found in this article, including but not limited
to text, trademarks, patents, logos, graphics and images (the "Materials"), are
the copyrighted works and other forms of intellectual property of Marcel
Downloaded by [b-on: Biblioteca do conhecimento online UP] at 09:27 17 June 2013

Dekker, Inc., or its licensors. All rights not expressly granted are reserved.

Get permission to lawfully reproduce and distribute the Materials or order


reprints quickly and painlessly. Simply click on the "Request
Permission/Reprints Here" link below and follow the instructions. Visit the
U.S. Copyright Office for information on Fair Use limitations of U.S.
copyright law. Please refer to The Association of American Publishers’
(AAP) website for guidelines on Fair Use in the Classroom.

The Materials are for your personal use only and cannot be reformatted,
reposted, resold or distributed by electronic means or otherwise without
permission from Marcel Dekker, Inc. Marcel Dekker, Inc. grants you the
limited right to display the Materials only on your personal computer or
personal wireless device, and to copy and download single copies of such
Materials provided that any copyright, trademark or other notice appearing
on such Materials is also retained by, displayed, copied or downloaded as
part of the Materials and is not removed or obscured, and provided you do
not edit, modify, alter or enhance the Materials. Please refer to our Website
User Agreement for more details.

Order now!

Reprints of this article can also be ordered at


http://www.dekker.com/servlet/product/DOI/101081DRT100001350

View publication stats

You might also like