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Compound Development with Design of Experiments or the

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 Special Reprint from
Magazine for the Polymer Industry RFP Rubber Fibres Plastics

Compound development with

design of experiments or
the GrafCompounder?

Volume 8, August 2013

03| 2013
 Computation of compounds

Compound development with design of pany, but hidden to him. With the amazing
number of recipes generated within a rubber

experiments or the GrafCompounder? company it is quite possible that searching

the archived recipes carefully would reveal
the newly created recipe being just a reinven-
H.-J. Graf* tion of the wheel. This is even more likely in
companies without standardisation of ingre-
dients for avoiding redundant raw materials.
The analysis of compounds in a database is limited to functions such as search-
Many chemists do not realise that often very
ing and identifying compounds. Programmes calculating formulations by applying
mathematical models of neural networks failed to predict a recipe with sufficient similar recipes are created, only differing in
accuracy. A programme using multiple linear iteration procedures can signifi- brand names of the ingredients used. Even
cantly optimise the accuracy of the prediction because it allows the identification if more advanced compounders would uti-
and elimination of corrupted data within the database. Such a method improves lise systematic approaches such as statistical
the data quality considerably. For checking the accuracy of the prediction two experimental design (DoE), some value will
examples have been used. For this exercise data sets from a statistical experimen- be lost. Typically, almost all the recipes used
tal design have been taken and the calculated results obtained by the prediction in a DoE are ignored or discarded when the
tool of the DoE programme as well as the programme GrafCompounder have been
optimum recipe has been found with that
compared to each other. It became apparent that the variance of the prediction
results of both programmes fell into the 95 % confidence interval. technique and the confirmation has been
successfully done. If an adjustment is still
necessary, the compounder will use the rec-
ipe as a starting point. The compounds from
1. Introduction pounds to manage process improvements, to the DoE are already archived meaning out of
increase process safety or to reduce manu- sight. This leads us to the question, how we
Many companies develop their own rub- facturing costs. can extract and utilise the value stored in old
ber compounds in house, typically building recipes, compound databases, or archives for
a large database of recipes over years of A typical rubber company is in operation future compound developments in order to
operation. These recipes naturally contain for several decades. It should not be a sur- save valuable time and money.
a set of ingredients and a set of properties. prise, that a company with a diverse rub-
ber article range has some 500 – 1 000 living In the recent past there were some inter-
New rubber formulations are often recipes (not forgetting the demand for spare esting approaches dealing with this problem.
created with varying methods. The method parts) and tenfold the number of laboratory In the literature some calculation methods
being mostly used is trial and error, common recipes taking into account the number of based on non linear regression were pub-
is still a one step at a time method and there recipes created during small scale evalua- lished [1 – 5] and a tool based on mathemati-
is an increasing number of statistical models tions. It can be reasonably assumed that all cal models of neural networks was available
for the design of experiments (DoE). these compounds have been manufactured on the market [6]. Extensive tests were done
at least once in a small laboratory mixer and with this programme, but predictions with
The development of a new compound can that their physical properties have been test- sufficient precision failed even with a large
originate from the demand for improve- ed too. We have to consider, that the cost database created and used for the query.
ment, validation of raw material properties, for mixing and testing of a single compound
or quality concerns. New recipes are often is worth approximately USD 500. This means The following is a description of a pro-
created based on existing compound for- that such a data base represents a substan- gramme having been developed recently. It
mulations for meeting new specifications, tial financial investment. But how often do applies a concept of the compositional ratio of
due to changing customer demands, or to we use this significant investment to our ad- a multi component material being determined
improve deficient products that suffer ser- vantage? What do we get in return? automatically by using a multiple linear itera-
vice life failures. New compound recipes are tion method (MLI) which is based on the linear
even created during the fine tuning of com- Whether a compounder takes a starting relationship between the material’s compo-
recipe from the literature of a material sup- nents and their physical properties [7, 8 – 12].
plier or uses an existing production formula-
tion, the industry standard is to create some
* Hans-Joachim Graf, recipes in the laboratory, always performing 2. Motivation for developing
hjgraf@cyg.net laboratory trials and evaluations followed the programme
Rubber Industry Consultant by plant trials. This procedure increases the
HJG Consulting, Bad Soden-Salmünster, number of recipes. Most likely a compounder The initial motivation for designing a new
Germany will not check whether his new compound is compound development programme was not
already available in the database of his com- prompted by the desire to recapture value

2 RFP 3/2013 – Volume 8

from previously developed formulations.
Rather it emerged due to lack of success
when working with a commercially available
compound development programme based
on a non linear approach like neural network
mathematics – as said above. The aim was to
reduce the amount of trial and error when
formulating and to foster a more scientific
approach to the creation of recipes. How-
ever, after more than one year of testing, it
was observed that the programme repeatedly
failed to predict accurately the properties of
the compound created. The database in use
was composed of compounds utilised on a
large scale and compounds created in a lab-
oratory environment at the same time. We
found out, that we were unable to predict a
compound with its properties to match the
target property values accurately enough,
which means within the 95 % confidence
interval. We concluded, that the database
contained too many faulty data. Just to give
an example: The tensile strength of some
compounds targeting at a high tensile was
much too low compared to the predicted val-
ues [6]. The confirmation experiments failed.
The mathematics of the programme seemed
to be intolerant regarding such faulty data.
The programme – as we would say - could
not learn, ignore or eliminate doubtful
data. If the ingredient property relationship
Fig. 1: Design guideline for developing the pro-
gramme GrafCompounder
• Calculation with linear relationships
 Most DoE show a linear model equation to be
sufficiently accurate.
 Math should be based on linear relationships,
but allow multiple small steps during calculations.
• Identification of faulty data in the compound database
should be easy.
• Programme should work correctly even with a smaller
database.
• Programme should be able to exchange data with all
types of calculation programme.
Fig. 2: Features of the calculation software Graf-
Compounder
The GrafCompounder is a:
• Spreadsheet software
 based on Java
 import / export function for communication
 allows automatic mixing of compounds and manual
mixing
 calculates profile of properties
 shows data composition of the results
 import / export of results
RFP 3/2013 – Volume 8
exhibited errors, the mathematics did not al-
low smoothing of the data compared to a
multiple regression analysis [13]. Since there
was no tool available for identifying faulty
data sets there was no chance to clean the
database.
The idea of building a database only with
compounds made within a statistic design of
experiment (DoE) would not eliminate the
problem, because the database entry would
be the property as measured but not cor-
rected via regression. Man is able to iden-
tify a property as an outlier in his analysis
of variance and may repeat the experiment
putting a new set of data in his database
for correction. The DoE programme, however,
will always use data fitted with its regression
equation just ignoring outliers.
If a multi component material with a plu-
rality of physical properties must be inves-
tigated and if linear relationships between
incorporated ingredients and corresponding
properties can be implied the analysis and
optimisation could be handled by a pro-
gramme much easier. Using linear relation-
ships should make the design of a material
composed of many components possible
with sufficient precision.
Looking into the old compounding tables
published in the past [7 – 12] you will find in
most cases a linear relationship for almost all
basic physical properties. Other publications
are showing that there is a linear relationship
found with the exemption of the tensile at
break. The latter could be true, because the
ingredients were varied within a much larger
range, which may cause such a non linear-
ity. We still can assume, that if changes of
ingredients are done in smaller steps, a linear
relationship will sufficiently describe the de-
pendency of properties on ingredients. Hav-
ing such a programme tool one would allow
a compounder to learn a lot about the real
value of his compound database.
Considering what has been mentioned
above a design guideline was created and
handed over to a programme developer
(fig. 1). The design guideline consists of few
requirements to meet the objectives of sim-
plicity, sufficient accuracy and ease of iden-
tifying the compounds in the database the
programme has used for the calculation of
the new compound. As a precondition the
programme should run on all personal com-
puters no matter which operating system
is in use. Data transfer/conversion should
be possible via copy/paste with almost all
standard spreadsheet software.
The answer to these objectives is a pro-
gramme called GrafCompounder. This pro-
gramme was extensively tested by the author
in all kinds of computer environments and
under all kinds of compounding challenges
like simple optimisation of physical proper-
ties up to more difficult tasks like surface
appearance of compounds (fig. 2).
3. Testing the GrafCompounder
To show the ability of the GrafCompounder
to predict a compound from any given data-
base, a comparison with DoE data was cho-
sen. The DoE programme uses a prediction
and optimisation tool to calculate a com-
pound. The result of this calculation can be
used for the purpose of comparing both cal-
culation methods. As DoE programme De-
sign-Expert was selected.
The difference between both tools:
Regression on the one hand, iteration on
the other, has some influence on the result
of course. The DoE tool uses statistical model
equations for data fitting and analysis within
the experimental design limits. It calculates
an area in between the boundaries. Inside
this area the properties are met in between
given limits. If all targets are matched the
probability is equal to 1, if not all targets
are matched the probability is less than 1.
The tool GrafCompounder works with dif-
ferent starting points, which are given by
the compound data in the database. It will
blend mixes mathematically and calculate
the properties as arithmetic average. A rat-
ing function estimates the distance from all
targets. Using multiple linear iteration and
minimisation of the difference between the
actual properties achieved and the desired
properties the targets are reached (fig. 3). As
soon as all the targets are met – that means
the rating function equals zero - the Graf-
Compounder yields one compound with its
3
 Computation of compounds

properties. In case of a plurality of bounda-
ries there are most likely conflicting targets.
In this case the rating function will show a
number different from zero with no further
decrease, indicating, that there is no better
solution possible. Regarding the purpose of
this comparison the question is, whether this
single point is inside the area of solutions
obtained by the DoE programme. At least it
should be inside the confidence interval of
the area of solutions.
3.1 Comparing DoE and GrafCompounder
by an oil/filler optimisation
As a first example a simple oil/filler DoE
was chosen, performed as a fractional facto-
rial design, to show basically how these tools
Now using the point prediction tool im-
plemented in Design-Expert we can set the
factors to the same values given by the Graf-
Compounder, analyse the responses, and
check, whether they are within the 95 %
confidence interval. Table 3 illustrates that
the results of both software systems are in-
side the confidence interval and within the
measurement errors of both methods.
As a first conclusion it is obvious that a DoE
programme, which is using a set of data and
calculating the responses by regression model
equations – either linear or non linear – will
output fitted and smoothed data. Calculations
with the fitted data will yield results, which
should be somehow different compared to a
software applying a stepwise iteration pro-
Ohm and Rajan Vara [14] has been analysed
using both tools. This DoE is dealing with
7 factors and needs 41 experiments to be
conducted resulting in a little larger data-
base of compounds than the example before.
The correlation of tensile and elongation
at break is linear as expected. Measured and
predicted data (fig. 5) indicate that there
must be a difference between the compound
calculated by the optimisation tool of De-
sign-Expert and by the GrafCompounder. The
Tab. 1: Oil/filler experiment – fractional factorial
design
Factor Name Unit Min Max
A CB 6630 phr 60 95

react on a limited set of data, which can eas- cess without any data fitting. Our expectation B CaCO3 phr 10 70

ily be overviewed by an experienced com- would be that there should be a characteristic C Clay phr 70 95

pounder. The factors of this DoE are shown difference but inside a small tolerance, which D Oil phr 70 95

in table 1. is indeed what we observed.

Tab. 2: Oil/filler experiment – conditions selected
Eleven experiments are necessary to per- 3.2 Comparing DoE and GrafCompounder for the optimisation
form the DoE with three replicates of the by a polymer/accelerator optimisa-
Response Limit
centre point. As responses for evaluation tion
the Mooney viscosity (MV), the scorch time Mooney viscosity MV 125 35 – 36 MU

at 125 °C (t5 – 125 °C) and the scorch time In the second comparison of a DoE and the Scorch time 125 °C t5 3.9 – 4.1 min

at 175 °C (t10 – 175 °C) were chosen. All GrafCompounder a DoE published by Robert Scorch time 175 °C t10 0.43 – 0.44 min

responses are significant using a linear re-

gression equation. The conditions selected
for the optimisation are given by table 2.

The optimisation with the software

Design-Expert software showed somehow Path 3

different results for the factors compared Path 4

to the GrafCompounder (fig. 4). The main
differences are the amounts of CB 6630
and CaCO3. To understand the difference
an additional condition was implemented
in the query of the GrafCompounder: The Path 2
amount of CB 6630 was set at 73 phr simi-
lar to the result of the optimisation with Path 5
Design-Expert. Now the results of the two
methods were much closer, the GrafCom-
Path 1
pounder had little less CaCO3 and clay for
its suggested compound. Are this differ-
ences important regarding the responses?
Analysis based on Report of results
To get an answer we used the function • measured data • recipe
point prediction of the software Design- • targets • all calculted physical
• weightings properties
Expert which is nothing else than a com- • rating functions show the distance  missing data ignored
pounding tool similar to the GrafCom- Fig. 3: between values and targets • show all recipes with their
Description of the mul- • iteration in small steps from different percentage used in an analysis
pounder but based on regression math- starting points
tiple linear iteration
ematics and limited to the set of data used • check of maximum agreement with
method applied by the the target
in the design. GrafCompounder

4 RFP 3/2013 – Volume 8

 reason is the difference between measured
and fitted data, which is shown in the cor-
Ingredients Unit DoE Optimisation GrafCompounder
relation graph.
CB 6630 phr 73 73
CaCO3 phr 68 61 In case of a DoE programme the calcula-
Clay phr 39 32 tion of compound properties will use fitted
Paraffinic oil phr 72 70 data, which do not deviate from the corre-
MV 125 MU 34 34.1 lation curve. The MLI method, however, will
t5 (125 °C) min 4.04 4.1 use the raw data instead. Knowing that the
t10 (175 °C) min 0.45 0.45 prediction of a compound by the DoE pro-
gramme compared to the result of a con-
Overlay Plot
70.00 firmation experiment is inside a 95 % con-
 fidence interval, one would expect, that a
64.00 MV: 34.008
 t5: 4.032 compound prediction by the MLI method
58.00 t10: 0.436 t5: 3.902
X1 72.16
using the GrafCompounder should also give
52.00 X2 60.84 a result within the 95 % interval.
t5: 4.100
46.00
t10: 0.439
B: CaCO3

MV: 34.300 MV: 36.000 As responses for the optimisation were

40.00 t10: 0.435
chosen: hardness from 65 Shore A to
34.00 70 Shore A, tensile from 11 MPa to 12 MPa,
Fig. 4: and elongation from 350 % to 400 %. The
28.00
Comparison of DoE opti-
misation and GrafCom- DoE optimisation within these bounda-
22.00

Optimisation area calculated with Design Expert
pounder quest results ries resulted in a polymer blend contain-
16.00 
Solution given by GrafCompounder with - top: table of results, ing 5.6 % ENB, 0.44 phr sulphur, 2.11 phr
the additional condition (CB 6630 = 73 phr) bottom: optimisation
10.00 DTDC, 1.00 phr MBT, 1.50 phr TBTD, 1.50 phr
graph with flag indicat-
60.00 67.00 74.00 81.00 88.00 95.00 ZDBC, and 1.50 phr DTP. The compound
A: CB 6630
ing responses from Graf-
Compounder properties of this composition were: ten-
sile = 11.2 MPa, elongation = 335 %, and
Tab. 3: DoE optimisation – comparison of the results by GrafCompounder and DoE point prediction hardness = 66.5 Shore A, which is indicated
by the flag in figure 6. Using the point pre-
Ingredients Unit DoE Optimisation GrafCompounder DoE Point Prediction
diction method instead of graphical optimi-
CB 6630 phr 73 73 73 sation yielded the same ingredient amounts
CaCO3 phr 68 61 61 as before.
Clay phr 39 32 32
Paraffinic oil phr 72 70 70 Keeping in mind the difference of the
MV 125 MU 34 34.1 34.2 ± 3 calculation methods in both programmes
t5 (125 °C) min 4.04 4.1 4.01 ± 0.25 the boundary conditions now were chosen
t10 (175 °C) min min 0.45 0.45 0.43 ±0.07 in a way that one could expect the same
values as indicated by the flag. The lower
Fig. 5: Correlation graph of predicted and measured data for tensile strength and elongation limits of the responses were set at exactly
these values for calculation: tensile from
16.00 Tensile 600.00 Elongation
11 MPa to 12 MPa, elongation from 350 %
14.00 500.00 to 400 %, and hardness from 65 Shore A
to 70 Shore A. After processing the data
Predicted

Predicted

12.00 400.00
with the GrafCompounder slightly differ-
10.00 300.00 ent results were obtained as shown in fig-
8.00 200.00 ure 7. The main differences observed were
the higher levels of ENB and sulphur and
6.00 100.00
a lower DTDC level to achieve the targeted
6.00 8.00 10.00 12.00 14.00 16.00 100.00 200.00 300.00 400.00 500.00 600.00
Actual Actual properties.
 Tensile at break is significant with linear model
• Sulphur has larger influence followed by DTDC and TBTD If the data were processed by the DoE
 Elongation is significant with quadratic model, but linear model is a sufficient fit
• Sulphur has the largest influence followed by DTDC programme with the same boundaries as in
 Hardness is sufficient significant with linear model as well the GrafCompounder there occurred a shift
• Main influence sulphur, DTDC
of the ingredient levels as displayed in fig-

RFP 3/2013 – Volume 8 5

 Computation of compounds

ure 8. The results are indicated by the yel-
low field (result DoE optimisation) and by the
flag (result GrafCompounder). But what is of
most interest: the sulphur level rise within
the DoE result while the ENB level is similar
to the value before and the DTDC level re-
mains high.
How close both solutions really are could
be demonstrated by using point prediction,
which means – as already mentioned above
– that the values calculated by the GrafCom-
pounder were put into the DoE software as
limits for calculation. For achieving the same
targeted property values the DoE still sug-
gested a lower amount of sulphur and a little
lower ENB level (fig. 9).
Anyhow, an experienced compounder will
notice, that a confirmation experiment in
the laboratory or even a large-scale test at
the plant will not reveal any differences out-
side the measurement error and the 95 %
confidence interval for the physical proper-
ties of both compounds. This leads us to the
second conclusion. The results of the two
very different approaches do not differ from
each other in reality at all.
4. Conclusion
A software using a multiple linear itera-
tion method is able to predict a compound
from unorganised data in any compound
database. Up to now such data could not
be utilised except for the selection or iden-
tification of a compound as a starting point
for further development work. The reason

Overlay Plot Fig. 7: Analysis by the GrafCompounder - results

1.50 and boundaries
  Factor values giving this results
• ENB: 5.58 %
• Sulphur – 0.44 phr Ingredients Result
• DTDC – 2.11 phr
• MBT – 1.00 phr A: ENB 6.5
1.20 • TBTD – 1.50 phr
• ZDBC – 1.50 phr B: DTDC 0.98
• DTP – 1.50 phr C: Sulphur 0.93
Tensile strength: 12.000
D: MBT 1
C: Sulphur

0.90
E: TBTD 1.51
F: ZDBC 1.33
G: DTP 1.45
Tensile strength: 11,214
Elongation at break: 335,106 Results
Hardness: 66,470 Elongation at break: 300.000 Tensile strength 11.5
0.60
X1 5,58
X2 0,44 Elongation at break 325
Tensile strength: 11.000
Hardness: 67.000 Hardness 67
Elongation at break: 350.000 Fig. 6: 
Boundaries
0.30
Graphical optimisation • Tensile strength-MPa: 11.5 – 12.0
5.00 6.00 7.00 8.00 9.00 • Elongation at break-%: 325 – 335
A: ENB
by DoE – factors indi-
• H-Shore A: 65 – 67
cated by flag

Fig. 8: Reprocessed data with the same boundary conditions for both software pro- Fig. 9: Comparison of predictions by GrafCompounder and Design-Expert for the
grammes same target properties
Overlay Plot
1.50
Ingredients Result GrafCompounder Result Design-Expert

A: ENB 6.5 5.45

Tensile strength: 12.000
Tensile strength: 11.536 C: Sulphur 0.93 0.88
1.20 Elongation at break: 306.017 B: DTDC 0.98 0.98
Hardness: 68.146
X1 6.50 D: MBT 1 1
X2 0.98 E: TBTD 1.51 1.51
Tensile strength: 11.498
F: ZDBC 1.33 1.33
C: Sulphur

0.90 G: DTP 1.45 1.44

Hardness: 67.489
Results
Elongation at break: 325.062
ZF 11.5 11.5
  Boundaries Elongation at break: 335.107
• Tensile strength-MPA: 11.5-12.0 ZD 325 330
0.60 • Elongation at break-%: 325-335 Hardness 67 67.5
• H-Shore A: 65-67 Hardness: 66.013
Note: Accelerators are preset!


The Design-Expert optimisation graph shows the location of the results 
Boundaries
as a yellow area, but GrafCompounder result is tagged with a flag. • Tensile strength-MPa: 11.5 – 12.0
0.30
5.00 6.00 7.00 8.00 9.00 • Elongation at break-%: 325 – 335
A: ENB • H-Shore A: 65 – 67

6 RFP 3/2013 – Volume 8

is, that a database, which contains such
unorganised data, cannot be transferred
in an organised form needed for a statistic
experimental design software as for instance
Design-Expert. A compound prediction with
a DoE software needs a set of data based on
planned experiments.
In this paper it could be demonstrated,
that processing the same compound data
either based on regression analysis (DoE
model equations) or based on multiple linear
iteration (GrafCompounder type processing)
leads to results being inside a 95 % confi-
dence interval and inside the fault tolerances
of the testing procedures applicable in the
rubber industry.
The disadvantage of the DoE software
is its inability to use data being unorga-
nised and outside the scope of an experi-
mental design. The advantage of apply-
ing a DoE programme is, that one always
gets a very good idea of dependencies
and interactions between ingredients and
properties. In addition the output of any
RFP 3/2013 – Volume 8
DoE will result in a very good compound
which can serve as a starting point for fur-
ther evaluation.
If a compound database is processed by
the GrafCompounder you will get a com-
pound together with its properties, only lim-
ited by the number of the data records con-
tained in the database. You will gain knowl-
edge about the influence of ingredients on
properties by simulating compounds without
even going into the laboratory, thus saving
time and money.
5. References
[1] US Patent 3,781,909 (1973), Edwin Ira Staerns
[2] European Patent Application 0 647 911 A2
(1994), Abe Akihito
[3] US Patent 6,411,945 B1 (2002), Yukio Nakajima
[4] US Patent 6,714,924 (2004),
Craig J. McClahnahan
[5] US Patent Application 0160114 A1 (2005),
Timothy D. Hunt
[6] Brett Kyle, private information 2001
[7] Robert O. Babbit, The Vanderbilt Rubber Hand-
book, Chapter 9, Compound Design, (1972)
[8] J. F. Turner, R. J. Kirschbaum, C. P. Louthan,
Profile of Cabot Carbon Blacks in Nitrile Rub-
ber, Technical Report RG-125
[9] E. C. McCaffrey, F. C. Church, F. E. Jones, Pro-
file of Cabot Carbon Blacks in Styrene Buta-
diene Rubber, Technical Report RG-129
[10] R. J. Kirschbaum, F. E. Jones, Profile of Cabot
Carbon Blacks in Natural Rubber, Technical
Report RG-133
[11] R. R. Juengel, Profile of Cabot Carbon Blacks
in Polychloroprene Rubber, Technical Report
RG-134
[12] D. C. Novakoski, Profile of Cabot Carbon Blacks
in EPDM Rubber, Technical Report RG-135
[13] A. C. C. Coolen, A Beginner’s Guide to Mathe-
matics of Neural Networks in: Concepts for
Neural Networks – A Survey, L. J. Landau, J. G.
Taylor (Ed.), Springer, Berlin, 1998, 13
[14] Robert F. Ohm, Rajan G. Vara, Timothy M.
Buckley, Sulfur Cure System Development for
EPDM Produced via Constrained Geometry
Catalyst Technology, Paper presented at the
Meeting of the Rubber Division, ACS, Indian-
apolis, IN, May 5 – 8, 1998
7
 HJG Consulting
Rubber & TPE &Coating Technology
Compounding Processing Education

Dr. Hans-Joachim Graf

Josef Leistenschneider Strasse 27
63628 Bad Soden Salmuenster
Germany

Contact:
Phone: +49 (0) 6056 209428 Cell +49 (0) 151 20006394
Telefax: +49 (0) 3222 1520721
www.grafcompounder.com
graf.hans-joachim@t-online.de

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