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FT-NIR Spectroscopy for quality and process control in Depth Filter
Sheets production
@
best@buchi
12
2001
Information Bulletin
Industrial Industrial
Industrial Industrial Industrial
FT-NIR Spectroscopy has many potential applications across
the whole production process of depth filter sheets. From
the identification of Raw Materials to the final product
qualification.
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FT-NIR Spectroscopy has many potential applications across the whole production process of depth filter sheets. From the
identification of Raw Materials such as different types of cellulose pads, white powdery fillers (e.g. Kieselgur = diatomaceous
earth, Perlite) or liquid chemicals such as wet-strength agents through to the final product qualification. In addition, NIR can also
determine physical parameters such as particle size, essential for the filtration behaviour, and determine parameters such as
moisture and permeability.
The efficiency and speed of NIR technology makes it possible to correct possible faults quickly in the production process. Waste
production can be minimised which is good for both the product profitability and the environment. Further tests have shown that
it is also possible to use NIR on-line in the production area, to monitor the concentrations of wet strength agents of the paper
suspension consisting of cellulose fibres, fillers and additives.
best@buchi
INDUSTRIAL 12 / 2001
Authors: Christoph Jansen (Bchi AG), Jrgen Ebert (FILTROX AG, P.O.Box, 9001 St. Gallen, Switzerland)
Introduction
Documented quality control plays a vital role in the production
of technical Depth Filter Sheets which are then used in areas
such as the Beverage and Pharmaceutical industries. Depth
filter sheets, typically up to several millimetres thick, are stacked
in plate and frame filter systems. They comprise the core of
stainless steel filter systems that can be up to several meters.
When a specialist in NIR spectroscopy becomes responsible
for production and quality control the total potential of NIR
often becomes more obvious than for any other economist or
engineer. This happened at the production plant described in
this paper. There were more than half a dozen different
applications in the whole process that could be handled using
NIR.
The application potential ranges from incoming raw materials
through production check on- or at-line to the quality control
of the final product.
An immediate potential for a quick return on the investment is
in the optimised drying process, finding the right production
belt-speed for an optimised throughput of the machines. This
can be combined with the right temperature profile for the
dryer for saving energy.
Experimental
The FT-NIR spectra are recorded using a Bchi FT-NIR
spectrometer NIRFlex N-400 based on a quartz wedge
birefringent interferometer. Unlike a Michelson interferometer
the beam coming from the source is collimated, polarised with
a 45 polariser, then split into two perpendicularly polarised
beams by using the birefringent nature of crystalline quartz.
Modulation is performed by continuously changing the thickness
of the lightpath by means of two quartz wedges. Finally, the
components of the two perpendicular light vectors are
combined using a second 45 polariser to produce the desired
optical interference
[1]
.
Thi s technol ogy produces a very stabl e and robust
interferometer essential for the rough environment of the
production plant.
The sampling accessory used to collect the data in this study
was a diffuse reflectance probe with a light fibre bundle to
illuminate the samples and to transport the light reflected from
the sample to the detector. Liquid samples were measured
using a transflectance probe. Fig. 1: Schematic view of the depth production process.
Fig. 2: The NIRFlex FT-NIR spectrometer used in the warehouse for
checking the raw material identity and quality.
best@buchi
INDUSTRIAL 12 / 2001
The chemometric computations are performed using Bchi
NIRCal software
[2]
for qualitative and quantitative applications.
As is typical for NIR applications, data pre-treatment such as
first derivative and normalisation were applied to spectra to
improve results and produce stable and portable calibrations.
Additionally, once calibrations were developed, spectra were
measured using a simplified user interface, required for
successful final application.
Results and discussion
Quality control of raw materials
Cellulose
Cellulose is used as the basis of the filter sheets and is obtained
from different woods with different properties such as fibre length
and stiffness. The cellulose is delivered as pads that are visually
difficult to identify other than by the attached label. However it
is important for the filter performance to use cellulose from the
correct kind of wood.
The NIR spectra were collected using a diffuse reflectance
probe, taking 3 scans at a resolution of 25 wavenumbers. The
identity is confirmed within a few seconds.
The chemometric method uses PCA, with 8 primary factors
for reconstructing the spectra and just 2 secondary factors to
distinguish the wood types. Figure 3 shows the cluster plot
with the tolerance radii for the different cellulose types.
Perlite/Kieselgur (Diatomaceous Earth)
Some of the production raw materials arrive as white powders.
Perlite and Kieselgur are the main filtering agents. They are
chemically identical and distinguished only by the particle shape
and structure. However there are many different grades of
Kieselgur and it is critical the correct grade is used to meet the
specifications of the filter sheets.
For this product type, some powdered filter aid materials are
added to the filtrate before filtration. Small particles in the
suspension stick to these filter aid materials and can be easily
separated in the filtering device to get a clear liquid.
The differentiation of the white powders was shown to be
possible. The clusters of some different types of Kieselgur (Type
A and C) are quite close but still separated with a reasonable
tolerance radius.
In all, 8 different powders need to be distinguished in this
production area. The spectra were measured using diffuse
reflectance via a fibre probe taking a 5 scan accumulation.
The determination is performed by PCA using 8 primary factors
for reconstructing the spectra and 4 secondary factors to
identify the differences.
Fig. 3: Clusters graphic showing the different types of cellulose which is
used as the Filter backbone.
The axis represent factors used to distinguish the cellulose types.
All cellulose types are clearly distinguishable.
Fig. 4: Factor-Loading plot (upper) and clusters graphic (lower) representing
the different powders used as raw material.
All powders are well distinguishable, even the two quite close Kieselgur
types A and C.
Fi g. 6 : Pl ot of the FT-NIR correl ati on of
Permeability (DZ) of the depth filter sheets:
Predicted versus true values.
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best@buchi
INDUSTRIAL 12 / 2001
Wet strength agent
Wet strength agents are aqueous emulsions of polymers or
resins added to the pulp. The suppliers specification for the
resin content is between 11 and 15 %. The resins are cured
through the drying process. The purpose of these wet strength
agents is to keep the final depth filter sheet from falling apart
when it becomes wet. The different types and qualities refer to
the specified different mechanical resistance and applications
of the depth filter sheets.
The correct amount of wet strength agent is measured online
in the pulp in the transflectance mode.
Moisture determination
The mixture is spread on a production belt where, during the
production process, water is drained off, then the paper is
dried and cut into the final size for use.
The drying process is performed in a dryer approximately 50 m
long at temperatures between 180 and 250C. Depending on
the recipe the paper enters the dryer with around 60-80%
water content. The course of the drying process is quite critical,
if the starting temperature is too high, this locks the pores and
the further drying is inhibited. On the other side initial temperature
is needed to start the curing process of the resin. With the
help of NIR-Spectroscopy it is possible to measure the moisture
profile in the paper along the dryer and find out the optimal
temperature profile. This helps save energy and costs.
The final product should have a specified moisture content of
around 1%. Thi s can al so be determi ned wi th NIR
Spectroscopy.
The filter sheets were measured using a diffuse reflectance
fibre bundle probe. The Reference method is a combination of
an infrared dryer and balance.
Figure 5 shows that the moisture concentration range can
easily be correlated with NIR measurements. The chemometric
method is PCR using 5 primary and 3 secondary factors.
Final product properties
One of the quality parameters for the final product is the DZ
(permeability value or flow rate). This value represents the
collective influence of different properties such as the type of
cellulose, filter agent (Kieselgur/Perlite) and the structure and
porosity of the depth filter paper.
It was found that DZ can be correlated with NIR as shown in
Figure 6. The plot shows the calibration for low permeability
values. The calibration is performed using a PLS algorithm taking
7 primary factors and 6 secondary factors. Correlation
coefficients of 0.973 for the calibration set and 0.979 for the
validation set can be
achieved.
I t i s possi bl e to
cover the whol e
product range with
just two calibrations,
one to determine
the range of high
permeabi l i ty, the
other to measure
the range of
rel ati vel y l ow
permeability.
Conclusion
As the data presented in this study demonstrates, NIR has
utility in a number of areas in a process environment. Preliminary
successful implementations include testing incoming raw
materials, optimisation of process parameters and finally product
performance testing. These capabilities combined with NIRs
speed and ease of use i l l ustrate the advantages of
implementing NIR in the production environment.
References
[1] J. Knecht, Design and Applications of a Near-Infrared Polarization Inter-
ferometer for Industrial Use, Mikrochim. Acta (Suppl.) 14, 769-771 (1997)
[2] www.ft-nir.com/nircal_software.htm
[3] Ch. Jansen, J. Ebert, FT-NIR Spectroscopy for quality and process
control in Depth Filter Sheets production, Submitted for NIR Publications,
Conference proceedings 2001.
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Fig. 5: Plot of the quantitative calibration of moisture in the paper: Predicted
versus true values. The reference method is an Infrared dryer with a balance.