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Methodology for the Determination of Stickies Concentration in Bleached Kraft

Recycled Pulp using and Interactive Image Analyzer

Chapter · January 1997

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Methodology for the Determination of Stickies Con
centration in Bleached Kraft Recycled Pulp Using an
Interactive Image Analyzer
S. Blais, P. Chabot, R. Gaudreault, and C. Tremblay
ABSTRACT
The methodology describes the various steps in
volved in the quantification of sticky contaminants
at room temperature with surface areas equal to or
greater than 0.08 mm2 using an interactive image
analyzer. Recycled wood-free papers are used in this
study. This description covers the method used to
prepare samples, i.e., pulp disintegration, 1aboia-
tory screening, suspension of contaminants, filtra
tion, drying, dyeing and characterization. The
various steps involved in image analysis are de
scribed. These include calibration, image acquisi
tion, discrimination, elimination of negligible
particles, particle filling, particle reconstruction,
particle selection, particle measurement, data clas
sification and results output. Finally, the repeat
ability of this method for the same operator and
different operators, within a 95% confidence level,
are also discussed.
KEYWORDS
Contraries, Deinked stock, Image analysis, Re
claimed papers, Stickies, Test methods.
Blais is Technical Representative, Allied Colloids, 11
Automatic Road, Brampton, ON L6S 4K6, CANADA.
Chabot is Process Engineer, Cascades Jonquiere Inc., 4010
Chemin St-André, PB. 1980, Jonquiere, PQ G7S 5K5,
CANADA.
Gaudreault and Tremblay are R&D Assistant Director
and Microscopist, respectively, R&D Cascades Inc., 471
Marie-Victorin St., Kingsey Falls, PQ JOA 1BO, CANADA.
Paper Recycling Challenge—Stickie8
INTRODUCTION
In the pulp and paper industry, the contamination
problem is a complex phenomenon of which a sig
nificant part is due to the presence of stickies. This
phenomenon can be compared to a moving target,
since the chemical nature of substances which are
at the root ofthis problem has been constantly evolv
ing in the last few years. One of the underlying dif
ficulties lies in the quantification and
characterization of such contaminants. Several
authors have documented methodologies used to
8J. One author CD has published
quantify stickies (1
1
a method which uses an image analyzer. It is speci
fied in the publication that the proposed method is
useful only as a quality control procedure for evalu
ating deinked pulp. It is therefore cliffiéult to com
pare it with the Cascades method since the latter
is used as a development and optimization tool
which is more time consuming. Some authors (4,)
have also characterized in detail the various types
of contaminants present in puips and finished prod
ucts.
Contaminants can be divided into two groups based
on their size (fi): macros (retained on the 150 .tm
Somerville slotted screen) and micros (not retained
on the 150 $.m Somerville slotted screen). Recent
publications (,jQ) refer to primary and secondary
stickies. According to the literature (a),primary
stickies are solid particles throughout the paper-
making process which become sticky under certain
conditions, and which result from “insufficient” dis
integration during pulping. Examples of products
giving rise to primary stickies are hot-melts em
ployed for book binding (which only stick during
drying and can induce spots and holes), and most
of the pressure sensitive adhesives (which begin to
stick at ambient temperature and are very difficult
to screen). Secondary stickies are much more com
plex particles because they result from physico
chemical changes which occur all along the paper
Page 49
manufacturing process, especially before the head
box. Initially, during pulping, some products are
completely or partially released in water, giving rise
to soluble or colloidal materials, respectively. These
soluble and colloidal materials can result from the
repulping of hydrodispersible adhesives, but more
often result from the repulping of coated paper (la
tex particles) as well as wood-containing papers (ex
tractable components), especially in alkaline
conditions. As soon as the pulp suspension is de
stabilized by the addition of cationic polyelectro
lytes, pH and temperature changes, etc., colloids
and/or soluble materials can be precipitated out of
the slurry producing secondary stickies (jo). The
methodology developed by R&D Cascades Inc. al
lows the determination of sticky particles concen
tration retained on the 150 jim Somerville screen
and which have a surface equivalent to and/or
. A smaller surface area could
greater than 0.08 mm
2 obtain a reproducible and statistically significant
) as a lower detection limit if
be used (e.g., 0.04 mm
2 result• can be varied.
the screening could be performed using a screen
with smaller slot width such as the Pulmac
Masterscreen which can be equipped with a 100
I.Lm slotted screen.
Application
This methodology can be applied to bleached kraft
recycled pulp, either at the wet end or on the fin
ished product. When testing a finished product, the
total procedure takes approximately one to two
hours. This time can vary greatly and may be sig
nificantly longer when testing is performed on pro
cess samples (screen feed, accepts, rejects, etc.). This
makes the actual procedure a development and op
timization methodology rather than a quality con
trol method.
PROCEDURE
Disintegration
Disintegration of wetlap pulp or diluted pulp is car
ried out using a standard British disintegrator at a
consistency of 2.0% (w/w) for five mm. Disintegra
tion of dry pulp or papers can be done with the same
technique provided they have been previously
soaked in tap water for at least 4 hr, preferably 24
hr, in order to ensure adequate defibering. This con
sistency was selected for practical reasons only and
future experiments should be conducted to evalu
ate the impact of consistency on the diameter of
the sticky particles once disintegration has been
completed.
Page 50
Screening
The pulp, at a consistency of 2.0% (w/w), is gradu
ally introduced into a Somerville vibrating screen
with 150 j.Lni slots so that total addition is done in
approximately five mm. The total screening time is
20 mm, which should be sufficient to pass all the
fibers for most pulp types. This procedure prevents
plugging of the screen slots. In general, the con
taminants that remain on the Somerville screen are
stickies, shives, plastic particles, wax particles, etc.
The quantity of pulp used has no critical bearing,
but usually varies between 100 and 150 g in the
case of a finished product. For the purpose of calcu
lation the exact quantity of pulp used must be
known. Finally, as mentioned in the literature (4),
the advantage of using a screen to concentrate con
taminants is that the amount of stock screened to
Suspension and Filtration of Contaminants
Contaminants remaining on the surface of the
Somerville screen are collected using a teflon
scraper, and then suspended with care in a 1000
ml teflon beaker containing approximately 500 ml
of deionized water at room temperature. Teflon is
used in order to prevent contaminants from cling
ing to the surface of the scraper and beaker during
transfer. The contaminant suspension is then fil
tered in a Buchner funnel using a Whatman wet
strengthened filter paper #111, 113, 114 or equiva
lent. However, this methodology carries a factor of
uncertainty, namely, the possibility that some par
ticles may stick together during the collectionlsus
pension step. Such uncertainty also exists during
the Somerville screening step. Therefore, further
experiments should be carried out in order to de
termine the presence of such a phenomenon, and
its impact, if any, on the repeatability and the va
lidity of the method used.
First Drying Step
The filter paper covered with the contaminants is
then place.d in an oven at a temperature of 105° ±2°
C for exactly 10 min. This step should allow the
sticky contaminants to adhere to the surface of the
filter paper as the filter surface dries.
Contaminants Dyeing
The contaminants are colored by immersing the fil
ter paper in a blue dye solution made from a solid
nonpolar organic dye trade name 15133 Oil Blue A:
Paper Recycling Challenge—Stickies
chemical name = Solvent Blue 36 (Color Index
Name) dissolved in heptane ( gil). Soaking time
generally varies between 5 and 10 sec. The blue dye
was ordered from Chemcentral Dyes and Pigments
Division, 13395 Huron River Drive, Romulus,
Michigan 48174. Afterwards, it is crucial to deli
cately wash the filter paper with contaminants in
a water bath, taking care not to dislodge the sticky
contaminants from the surface of the filter paper.
This step is necessary in order to make the stickies
stand out, i.e., blue sticky contaminants on a white
background, for better resolution of the image dur
ing the analysis. It is important to note that light
plastic contaminants may float upon washing.
These contaminants, not beiig stickies, are nor
mally discarded before the analyses.
Second Drying Step
The filter paper with the colored contaminants is
placed in an oven for exactly two mm at 105° ±2° C.
Characterization
The characterization step is very critical since other
particles besides stickies are colored at room tem
perature. For example, poor washing may some
times result in colored and/or partly colored shives,
plastic films, waxes, etc. Therefore, it becomes im
portant to make sure that only sticky particles are
being analyzed. The characterization of the con
taminants is done at room temperature. This pro
cess is carried out with a microscope and a metallic
needle. Each contaminant identified as “tacky” is
circled with a pencil mark and later analyzed.
From a theoretical point of view, it may be men
tioned that some contaminants which do not show
up as sticky particles at room temperature can be
come so when the plant’s operational temperature
is reached. Though this hypothesis is sustainable
in an operational context, it is not possible to pre
dict which contaminants will become sticky at
higher temperatures as too many variables come
into play, i.e., chemical nature, glass transition tem
perature, time spent at that particular temperature,
etc. Moreover, in pulps analyzed up to this point
(wood-free types), the contaminants that were de
fined as sticky particles at room temperature rep
resented the bulk of contaminants that were colored
by the blue nonpolar dye.
Sometimes a superposition of particles can occur.
Such a phenomenon is somewhat totally, or at least
partially, resolved by manually dislodging the ag
glomerated particles. It would be possible to cor
Paper Recycling Challenge—Stickies
rect such anomalies through programming by re
constructing both particles from their visible sur
faces; however, the phenomenon as well as the error
factor that can result from such a manipulation of
the data should be studied further.
It must be mentioned that waxes are not analyzed
by this method because their melting point is too
low, which seems to have a significant impact on
the surface of the particles. Moreover, the varia
tion in the coloration level of this type of contami
nant using the nonpolar dye could represent a
significant source of errors. The same holds true
for plastic films which are not considered since there
is a wide variation in the coloration level for this
type of contaminant and also because they might
be partially or totally lost during the dyeing step
(gentle washing). Finally, ink-like particles will be
recorded as long as they are sticky at room tem
perature. For example, laser or xerographic inks
which have been exposed to a solvent and have soft
ened could be recorded.
Image Analysis
Image analysis is carried out using a Kontron Elec
tronics interactive image analyzer distributed by
Zeiss. The image acquisition is done with a Hitachi
color video camera which is mounted on a micro
scope. The images are then transmitted to a com
puter that stores, processes and measures the
various characteristics of these images according
Figure 1: Structure of the stickies surface measurement
macros.
I CALIBRATION I
IMAGE ACQUISITION I
I DISCRIMINATION I
IELIMINATION OF NEGLIGIBLE PARTICLES
I PARTICLE FILLING I
PARTICLE RECONSTRUCTION I
r PARTICLE SELECTION I
I PARTICLE MEASUREMENT I
DATA CLASSIFICATION I
I RESULTS OUTPUT I
Page 51
to the logistics described in Fig. 1. The microscope
lighting system uses reflected light and an optical
fiber peripheral lighting system which is controlled
by a dimmer.
Calibration
The level of magnification of the microscope is ad
justed in order to obtain a maximum resolution by
placing a large sticky under the objective and ad
justing the microscope so that the sticky fills up
approximately 50% of the area under observation.
The scale is then calibrated using a micrometric
ruler. The scale calibration is done for the x and y
axes respectively, in order to correct any possible
distortion of the optical system. At the program
ming level, the scale calibration is carried out in
teractively by pointing the ends of the micrometric
ruler and by entering the desired units as well as
the pointed distance. The computer then calculates
a length per pixel ratio. The result obtained is then
used as a reference for future calculations. Typical
resolutions which have been used so far and seem
appropriate vary from 5.26 x 5.26 p.mlpixel to 6.90
x 6.90 p.m/pixel.
Image Acquisition
The image transfer from the camera to the com
puter is usually the first step in the image analysis
process. In the case of the present methodology,
image processing is done in black and white, i.e., in
accordance with the
shades of grey that are
subdivided on a scale
from 0 (which stands for
100% black) to 255
(which represents the
• 100% white) for each
pixel (Fig. 2). It is also
necessary to take one
image per contaminant
particle rather than to
make a full scan of the
Figure 2 Grey level scale, sample at once.
Image Discrimination
This process is aimed at recognizing the particles
that are being targeted. At this stage, the operator
interactively selects the range of grey level that will
determine which pixels are to be selected. Those
pixels will be set to a grey value of 0 (black). Any
other shade will automatically be eliminated, as it
will be considered as background (pixels set to
Page 52
lb
a
Figure 3: Initial image. Figure 4: Discriminated image.
white). The next steps are then performed on a bi
nary image (black and white) (Figs. 3 and 4).
Image Alteration
The next three operations are carried out automati
cally and are aimed at correcting the surface of ob
jects which has been altered by external factors.
Elimination of Negligible Particles
Particles with a negligible surface (10 pixels) are
often derived from the presence of residual dye
lumps or by the quality of the lighting or electronic
noise. Consequently, ghost particles are eliminated
right from the beginning. It must be noted that the
particles being analyzed are of a much greater or
der of magnitude (equivalent diameter of 319 to
2523 p.m) than those of ghost particles (Figs. 5 and
6).
V
Particle Filling
Because of their tackiness, one can very often ob
serve particles of a smaller size and of a different
shade of grey adhering to the surface of larger stick
ies (Fig. 7). The surface of a larger sticky being com
puted is then falsified because the varying shades
of grey of the smaller adhered particles are inter
preted as small white surfaces. Such an anomaly
can be corrected by filling in these white spots. At
the programming level, filling is done by automati
cally adjusting pixels with a maximum level of grey
shade (255) that are surrounded by pixels with a 0
grey shade (binary image) to a grey shade value
equal to 0 (Figs. 8 and 9).
Particle Reconstruction
Very often, the sticky is intermingled with one or
several fibers which produce a different shade of
grey. In terms of image recognition, this translates
into a series of various small particles (Figs. 10 and
Paper Recrycling Challenge—Stickies
 11) instead of a single large particle, thereby falsi
fying the statistics for this sample.

‘4
Figure 5: Discriminated im- Figure 6: Result of elimina
Such an error is corrected through object dilation
(expansion of the surface through the addition of
pixels until a complete filling is obtained). Once this
is done, the operation is reversed and the particle
is eroded to its initial surface (Figs. 11 to 13).

Specific Cases (Interactive Tracing)

age with negligible par-
tides.
Figure 7: Particle before
filling.
tion of negligible particles.
Figure 8: Particle before filling
without background.
Particle Analysis
In some specific cases, the surface that is recognized
by the image analyzer does not reflect reality. This
can result, for example, from a crossing of the pen
cil mark made by the operator with the particle
(Figs. 14 and 15), or from the complete filling of
the circle traced around the particle (Figs. 16 and
17). In these rare cases, a mitigative measurement
is available, i.e., the operator interactively circles
the area to be selected, taking care to eliminate any
undesirable object. Such an exceptional procedure
requires time and caution. Once this procedure is
performed and the surface of the particle is recon
structed, it then becomes possible to measure the
actual characteristics of the particle (Figs. 18 to 20).

Once objects have been selected, they can be ana

lyzed. In the case of stickies, the following param
eters are generally computed: surface area, number
of contaminants, equivalent diameter, circulatory
shape factor and “DMIJD” ratio. Various data
analyses can then be carried out, such as the clas
sification of results by surface area, equivalent di
ameter, etc.

So far, the most appropriate method for preseüting

results seems to be the surface of the contaminant
Figure 9: Image after filling Figure 10: Initial picture.
process.
for a fixed quantity of pulp, e.g., mm2 of contami
nants per 150 g pulp. Obviously, the reference mass
of pulp is not a crucial factor, as it can vary when
ever necessary, based on the initial concentration
* I. of sticky particles in the pulp sample.

Repeatability of Image Analysis

Repeatability of the image analysis for the same

0 operator and different operators within a 95% con
fidence level was calculated using the method sug
gested by the Direction des laboratoires, Ministère
de l’Environnement, Gouvernement du Québec (fl).
pp The repeatability for the same and different opera
Figure 11: Identification of Figure 12: Image with fill- tors was determined from ten measurements per
particle without image cor- ing and dilation. sample, only taking into account image analysis (see
rection.
Appendix for repeatability equation), i.e., they ex

Paper Recycling Challenge—Stickies

Page 53

Figure 13: Resulting image
after particle erosion.
Figure 15: Resulting image,
particle and pencil mark
combined.
Figure 17: Resulting image,
circle filling causing an
identification error.
Figure 19: Selection of an
area of the initial image.
Page 54
Table 1. Repeatability of Image Analysis. ;
Total surface Repeatability* Repeatability
of stickies Same Operator Different Operators
sample - Same Conditions Same Conditions
,,
(mm %) (%)
, 4.3 j
485 29 *
-8.87 3.6 .Zc4.:’ 8.77
t’
Figure 14: Initial image,
particle and pencil mark.
dude any error related to the method used for pre
paring samples (Somerville screening, suspension
of contaminants, ifitration, drying, dyeing and char
acterization).
The repeatability obtained on the image analysis
only seems to be good considering this type of
method. An extension of this methodology has been
developed for the determination of stickies concen
tration in recycled 0CC and liner pulp (iZ. The
method described has better repeatability than the
ones reported here, and is nearly identical except
Figure 16: Initial image with that the image analysis is performed with true color
pencil circle. processing. This adaptation was necessary because
of the characteristics of the Somerville rejects,
where a lot of brown shives, waxes, plastic films
and stickies are present. The true color processing
gives the ability to measure the blue surface area
v.. on either a brown, white, or otherwise colored ma
trix.
Therefore, further experiments are required in or
der to determine the statistical performance of the
global method (sample preparation plus image
analysis).
Figure 18: Initial image.
CONCLUSIONS
The methodology developed allows the quantifica
tion, with sufficient precision, of the stickies found
in bleached recycled pulp (wood-free type), and
should be considered as a development and process
optimization method. However, further experiments
should be carried out in order to optimize the meth
odology, so as to:
• Determine the impact of disintegration time on
the distribution of the sticky particles’ equivalent
diameter.
Figure 20: Image after • Determine whether sticky particles adhere to
correction. gether during the Somerville screening and the con
taminant collection/suspension steps.
Paper Recycling Challenge—Stickies
• Investigate the phenomenon related to superposed
particles, if any, and the potential error that could
result from such a phenomenon.
• Improve the overall repeatability of the method
by carrying out true color processing.
• Determine the global method’s overall repeatabil
ity (sample preparation plus image analysis).
• Compare this methodology with others.
• Since Pulmac screening could reduce the analy
sis time by approximately 20 mm, it seems appro
priate to compare the results obtained with the two
apparatuses and eventually substitute the
Somerville by the Pulmac as long as the repeatabil
ity is acceptable.
ACKNOWLEDGMENT
The authors would like to thank Mr. Louis Sénéchal
(Mill Manager), Mr. Marcel Lambert (Production
Manager) and Mr. Maurice Theberge (Laboratory
Supervisor) of the plant at Desencrage Cascades, a
Division of Rolland Inc., for their financial, techni
cal and operational support. We also wish to thank
Dr. Martin P. Pelletier and Dr. Christian Lauzier
for the valuable technical information as well as
Mrs. Pierrette Lamontagne for the preparation of
this document. Finally, we would like to thank Mr.
Rémi Beaulieu (Mill Manager) of the plant at
Desencrage CMD Inc. for his financial support.
APPENDiX
The repeatablility for the same operator has been
determined on three pulp samples coming from
three different mills and having a total stickies sur
face area of 1.50, 4.85, and 6.87 mm
. The statisti
2 vey. Prog. in Paper Recycl. 2 (3): 80-84 (May 1993).
cal equation used, assuming a normal curve
distribution, is:
Repeatability = t (0.95. n-i) x S.D.
.‘Jn
where: n=number of readings
(N.B.: n =10 in these cases)
t (0.95, n-i) = from Student’s table
S.D. = Standard deviation
Paper Recycling Challenge—Stickies
Table 2. Example of repeatability
calculation for the same operator.
Analysis Wetlap pulp Breakeyville
Area (mm
)
2
1 1.45
2 1.51
3 1.57
4 148
5 1.66
6 1.44 .••‘.‘
7 1.43
8 1.67
9 1.42
10 1.44
Average 1.51
Standard deviation 0.09
Repeatability 4 25%
LITERATURE CITED
1. Forester, W. Methods for the detection of stick
ies in pulp. Contaminants Problems and Strategies
in Waste Papers Seminar, pp. 161-168, Cincinnati,
OH (Apr. 28-30, 1992)..
2. Knight, P.A. Revised standard: Stickie determi
nation method. Beloit Corp. (Dec. 3, 1980).
3. Jean, M.; Nguyen, X.T. Quantification and re
moval of stickies from 0CC waste papers. CPPA
Research Forum on Recycling, pp. 61-69 (Oct. 5-7,
1993).
4. Staff. Methods to quantifr stickies: A mill sur
5. Ouellette, A.J. Troubleshooting for stickies us
ing the Doshi method. Prog. in Paper Recycl. 4 (2):
85-88 (Feb. 1995).
6. Doshi, R.M. Quantification of stickies. Prog. in
Paper Recycl. 4 (2): 103-106 (Feb. 1995).
7. Darlington, W.B.; Blair, W.R. Quantification of
thermoplastic stickies with an image analyzer. Prog.
in Paper Recycl. 4 (3): 68-70 (May 1995).
Page 55
8. Matzke, W.; Selder, H. Additional benefits from
pressureless high consistency dispersing of second
ary fiber stock. Proc. TAPPI Pulping ConL, Book 3,
TAPPI Press (Oct. 1986).
9. Carré, B.; Brim, J.; Galland, G. The incidence of
the destabilization of the pulp suspension on the
deposition of secondary stickies. Proc. 3rd Research
Forum on Recycling, pp. 187-197 (Nov. 20-22, 1995).
10. Carré, B.; Brim, J.; Galland, G. Comparison of
two methods to estimate secondary stickies con
tamination. Prog. in Paper Recycl. 5(1): 68-72 (Nov.
1995).
11. Gouvernement du Quebec, Ministère de
l’Environnement, Direction des laboratoires,
“Protocole de definitions et conventions pour la
flabilité et la validation d’une méthode d’analyse
en physico-chiinie”, May 1993 Math. 1.1. (In French)
12. Fillion, M.; Gaudreault, R.; Roy, B. Methodol
ogy for the determination of stickies concentration
in recycled 0CC and liner pulp using interactive
image analyzer in real color processing mode. Un
published work (March 23, 1995). (In French)

Received for Review November 18, 1996

Accepted December 19, 1996

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