Abstract-- This work is aimed for the detection of fault occurred

in the semi-batch reactor, which treats chromium sludge, at

high sludge flow rate. Multivariate Statistical Process Control
(MSPC) techniques and Principal component analysis (PCA)
were applied to the simulated data for monitoring. In this work,
an attempt is made by employing Lanczos symmetric
tridiagonalization means for the determination of largest
principal components instead of classical methods. Using
established PCA model from normal operating condition
batches, semi-batch reactor is monitored for specified time
period in online fashion. T
2
statistic was computed for each
sample in order to identify abnormal scenario. The results have
shown that the fault is successfully detected.
Keywords: Fault location, fault diagnosis, principal component
analysis, process monitoring.
V. INTRODUCTION
he effect of unknown disturbance on process, failure of
sensors, unsatisfactory performance of control, violation
of the operational constraints and failure of valve are
predominant sources that lead to abnormal situation. An
abnormal situation has profound effect on final product
specifications, plant safety and economy. To bring the process
again to normal situation, fast detection and analysis of fault
must be done. Though several techniques are available for
fault detection, multivariate statistical process control
technique, Principal Component Analysis (PCA), has proven
as a promising approach for monitoring of chemical and
bioprocesses. PCA provides data dimensionality reduction by
screening out insignificant variables from process, outlier
detection and feature extraction. Since PCA has the benefit of
comparing current process status with reference (desired)
state, it was applied on batch and continuous processes with
help of Hotelling's T
2
and Squared Prediction Error (SPE) [1,
2]. Martin et al. studied the application of MVSPC techniques
and the effect of different confidence bounds for monitoring
batch methyl methacrylate polymerization reactor [3]. Lennox
et al., Gunther et al. and Chiang et al. have analyzed the
faults occurred in industrial fed-batch fermentation using
Multi-way PCA and Multi-way Partial Least Squares [4-6].
T
S. K. Damarla is Ph.D student in the Department of Chemical Engineering,
NIT Rourkela, Rourkela, Orissa, India (e-mail: seshu.chemical@gmail.com).
M. Kundu is Associate Professor in the Department of Chemical Engineering,
NIT Rourkela, Rourkela, Orissa, India (e-mail: mkundu@nitrkl.ac.in).
When process operating point is changing frequently, static
PCA cannot reflect the process variations. Li et al. proposed
recursive PCA which updates PCA model corresponding to
variation in process parameters [7]. Several reports regarding
the application of PCA in chemical and bioprocess can be
found in open literature.
The recycling of tannery waste, Chromium sludge, uses semi-
batch reactor to recovery Chromium (III) sulphate [8]. To
process large amounts of sludge, a high temperature is to be
maintained. However, the reactor has certain operational
constraints; maximum reactor temperature should not exceed
100
o
C and total mass in the reactor, which is limited by the
height of the coolant double wall, must be below 2450 Kg [9].
Violating these limits induce the process to deviate from the
specified operating condition. Therefore, monitoring and
control are vital to ensure the safe operation [10, 11].
This work is intended to detect the fault generated in semi-
batch reactor, processes tannery waste, at high sludge flow
rates. The rest of the paper is organized as follows. A
complete theory of PCA is given in section 2. Section 3
describes the process and generation of fault. Results are
presented in section 4. Eventually conclusions and significant
findings are bestowed.
II. PRINCIPAL COMPONENT ANALYSIS
A. PCA Model
Batch data, X , can be visualized as three dimensional data
(IJK); I-batch, J- variables and K- time instances. It can be
unfolded as variable wise (IKJ) or batch wise (IJK). In this
work, variable wise unfolding is considered. Usually process
measurements are in different magnitudes. Prior to the
development of PCA model, the data must be auto scaled in
order bring all measurements in one range. After scaling the
data, correlation matrix is calculated as per (1). There are
several techniques available for the determination of largest
principal components to be retained. Besides these methods,
Lanczos symmetric method is useful in determination of
significant principal components [12, 13]. This method is
precious where the large number of process variables
considered in analysis. Applying Lanczos method on
correlation matrix yields tridiagonal matrix as shown in (2),
1 1
m m
,
having less number of dimensions than
m m
R

.
This algorithm, given in Table 1, is terminated when the
eigenvalues of 1 1
m m

are approximately equal to the

eigenvalues of
m m
R

. The eigenvectors, V , and
eigenvalues, D, of 1 1
m m

can be computed according to

(3). The projection of Lanczos vectors, L , on eigenvectors
yields PCA loading matrix which is holding important
information about process variables. The process is identified
in subspace by projecting the original process data, X , onto
the loading matrix. The variation, not captured by PCA, is
left in residual matrix E .
1

n
X X
R
'
(1)
where n is number of samples.
Monitoring Semi-Batch Reactor Using Principal
Component Analysis
S. K. Damarla and M. Kundu
1

,
_

1 1
1
1 1
1
1
2
2 2 1
1 1
'
0 0
0 0
0
0 0
m m
m
m m
RL L

(2)
) ( eig ] D , V [
(3)
V P
(4)
XP T
(5)
' TP X E
(6)
Table 1: Lanczos Symmetric Tridiagonalization
0
r is given,
0 0
r
while (trace(

)/trace(R)) )
1
1

j
j
j
r
q

j j
Rq u
1 1

j j j j
q u r ( 0
0
q )
j
T
j j
r q
j j j j
q r r
) (
1
j
T
v
j
v
v j j
r q q r r

j j
r
Forming tridiagonal matrix,

, with
j

and
j

End
To authenticate whether the process is running safely or
abnormally, the process must be monitored. This will be
accomplished by projecting new measurement vector onto
PCA model. The corresponding score and residual vectors
can be calculated using the following equations. The
statistical metrics of every sample will be computed according
the formulae presented in the next section.
( )
1
P P P x t
'
new new
(7)
' P t x e
new new new

(8)
B. Hotelling's
2
T
and
Q
The statistical metrics,
2
T
&
Q
, are helpful in knowing
the process status.
2
T
is a measure of multivariate distance
of each data point to the centre of the PCA model whereas
Q
-statistic finds the variation that has not captured by PCA
model. The scalar value of
2
T
statistic can be computed
from the next form,
'
new
'
new
t )
n
T T
( inv t T
1
2

(9)
If the data follows normal distribution, the upper limit of
2
T
is defined in the next equation by Fisher-Snedecor
distribution with level of significance.
) m n , m ( F
) m n ( n
m ) n (
T
1 1
1
1
2
2
1

(10)
where
1
m is largest principal components obtained from
tridiagonal matrix.
Q
statistic is defined below as sum of squares of residuals.
The upper limit of
Q
can be calculated by (12). An
abnormal event occurs if any of statistical metrics violates the
limit.
'
new new
e e Q
(11)
o
h
o o o
h h c h
Q
1
2
1
2
1
2
1
) 1 (
1
2
1
1
]
1

+ +

(12)
where

m
m j
i
j i
1
1

,

,
_

2
2
3 1
3
2
1

o
h and

c is the
value of the normal distribution with level of significance.
III. CHROMIUM SLUDGE RECYCLE PROCESS
Fig. 1 represents the treatment of chromium sludge in semi-
batch reactor surrounded by a double walled cooling jacket to
minimize excess temperature. The height of the cooling wall
limits the reactor working volume to 21166
3
m
. Therefore,
allowable mass in the reactor is 2450
Kg
. The reactor is
initially charged with aqueous potassium dichromate and
aqueous sulphuric acid. The recycle sludge is slowly added to
the reactor where it reacts with aqueous solution to produce
chromium (III) sulphate. Considerable heat liberated from the
exothermic reaction, takes place in the reactor, causes
increase in the reactor temperature. On the other hand, the
reactor should not be operated above 100
C
o
. Disobeying
the operation constraints lead to abnormal situation.
Fig. 1: Semi-batch reactor
The process is represented by dynamic model comprising of
non-linear differential equations from (13) to (16). Runga
Kutta fourth order technique was used to simulate ODEs at
B
m m a c T , , , ,
C V C
C T F , ,
VP V
T m ,
Sludge Chromium
FK F
T m ,
2
different operating conditions. Since steady state is
accomplished only before sludge enters the reactor or at the
end of reaction, process exhibits dynamic nature throughout
the reaction. Table 2 provides the list of values of the
parameters used in model. The initial conditions together
with physical limits and steady state values are presented in
Table 3. By varying the sludge flow rate,
FK
m , from 0 to 2 (
sec
Kg
), 11 batches data (NOC) under normal operating
condition were collected. At 3
FK
m , mass inside the
reactor was more than 2450
Kg
. Accordingly reactor
temperature was raised above the operating limit 100
C
o
.
Hence, fault was generated in the process. 12
th
dataset is
having the measurements of the faulty batch. Figs 2 & 3
depict the dynamic behavior of mass and temperature when
abnormal situation occurred.
FK
m
dt
dm

(13)
FK
FK FK
ka
m
m
dt
da

(14)
( )
R
V
R
FK r
R
FK FK FK
mC
T T KS
C
ka H
mC
T C m
dt
dT
+

(15)
V VR
V
V VR
V V
V VR
VP V V V
C m
) T T ( KS
C m
T C m
C m
T C m
dt
dT
+
(16)
Table 2: Values of parameters
factor l exponentia pre , A
219.
6
)
mol
J
( energy activation , E
2996
8
)
K mol
J
( t tan cons gas , R
8.31
4
)
K Kg
J
( sludge of heat specific , C
FK
4400
)
K Kg
J
( coolant of heat specific , C
V
4118
5
)
K Kg
J
( coolant of heat specific , C
R
4500
l (Kg) double wal reactor ss in the coolant ma , m
VR
220
)
s
Kg
e ( ss flowrat coolant ma , m
VR
1
)
Kg
J
reaction ( of heat , H
r

139235
0
)
K m
W
t ( coefficien conduction , K
2
200
) area(m urface transfer s heat , S
2 7.36
e (K) temperatur sludge input , T
FK
293.
15
e (K) temperatur coolant input , T
VP
288.
15
Table 3: Steady sates and physical limits.
Initial conditions Operational
constraints
Steady state
condition
1811 ) 0 ( m
0 ) 0 ( a
FK

o
K 15 . 323 ) 0 ( T
o
V
K 15 . 293 ) 0 ( T
2450 m <
o
K 373 T <
0 m
FK

0 a
FK

VP
T T
VP V
T T
0 100 200 300 400
1000
2000
3000
4000
5000
6000
7000
8000
time (sec)
m
a
s
s

i
n

r
e
a
c
t
o
r

(
K
g
)
Fig. 2: Total mass profile in the reactor when fault occurred.
0 100 200 300 400
200
400
600
800
1000
1200
time (sec)
t
e
m
p
e
r
a
t
u
r
e

(
K
)
Fig.3: Temperature profile when fault generated
3
IV. RESULTS
PCA model was built using 11 NOC batches obtained from
normal operation of semi-batch reactor at low and moderate
sludge flow rates. This PCA model is being the reference to
the measurements of unsuccessful batch. Using Lanczos
method, a tridiagonal matrix of fewer dimensions was
determined. The largest principal components determined by
cumulative percent variance (CPV) state that the mass in the
reactor and concentration of sludge are good enough to
represent the process in subspace. The result of CPV method
was depicted in Fig. 4. The significant principal components
shown in Fig. 5 confirmed that the Lanczos method is
alternate to the existing methods used for the selection of
number of principal components. The upper limit of T
2
statistic of PCA model was determined. Every new
measurement vector of process is projected on reference PCA
model to calculate T
2
statistic which is plotted in Fig. 6. At
40
th
time instant, T
2
statistic crosses the upper limit that
indicates the occurrence of fault in the process.
1 2 3
0
0.5
1
1.5
2
2.5
3
3.5
principal components
e
i
g
e
n
v
a
l
u
e
s
Fig. 4: Selection of PCs using Cumulative Percent Variance
1 2 3
0
0. 5
1
1. 5
2
2. 5
3
3. 5
principal compone nts
e
i
g
e
n
v
a
l
u
e
s
Fig. 5: Selection of PCs using Lanczos Method
V. CONCLUSION
Principal component analysis was applied to batch data
obtained by simulating the semi-batch reactor at different
sludge flow rates. At high sludge flow rate, process variables
did not obey the operational constraints that led to faulty
situation. To detect the fault, statistical metric, T
2
, was
computed online by projecting the new observation vector
onto the reference PCA model developed from 11 NOC
batches. The significant principal components, process
variables, were computed by Lanczos method. It is found that
Lanczos method has ability to find largest number of
principal components (variables) in comparison with CPV. Its
use is more beneficial when several variables are involved in
the analysis.
0 50 100 150 200 250 300 350 400
10
0
10
1
10
2
10
3
samples
T
2

s
t
a
t
i
s
t
i
c
upper
limt
Fig. 6: Fault detection using PCA
VI. REFERENCES
[1] P. Nomikos, J. F. Macgregor, "Multivariate SPC charts for monitoring batch
process," Technometrics, Vol. 37 (1), pp. 41-59, 1995.
[2] D. G. Alvarez, Fault detection using principal component analysis (PCA)
in a wastewater treatment plant (WWTP), in Proceedings of the
International Students Scientific Conference, 2009
[3] E. B. Martin, A. J. Morris, M. C. "Papazoglou, C. Kipparissides, Batch
process monitoring for consistent production," Computers chem. Eng, Vol.
20, pp. 599-604, 1996.
[4] B. Lennox, G. A. Montague, H. G. Hiden, G. Kornfeld, P. R. Goulding,
Process Monitoring of an Industrial Fed-Batch Fermentation," Biotechnol.
Bioeng, Vol. 74 (2), pp. 125-135, July 20, 2001.
[5] J. C. Gunther, D. E. Seborg, J. Baclaski, "Fault Detection and Diagnosis in
Industrial Fed-Batch Fermentation," in American Control Conference,
2006.
[6] L. Chiang, A. Kordona, L. Chewb, D. Coffey, R. Waldron, T. Bruck, K.
Haney, A. Jenings, H. Talbot, "Multivariate analysis for quality
improvement of an industrial fermentation process," in 7th International
Symposium on Dynamics and Control of Process Systems, Cambridge,
Massachusetts, USA, July, 2004
[7] W. Li, H. H. Yue, S. Valle-Cervantes, S. J. Qin, "Recursive PCA for
adaptive process monitoring," J. Process Contr., Vol. 10, pp. 471-486,
2000.
[8] L. Macku, "Control design for the preparation of regenerate for tanning,"
Ph.D. Thesis, Dept. Electronics and Measurements, UTB, Zlin, 2003.
[9] F. Gazdos, L. Macku, "Analysis of a semi-batch reactor for control
purposes," in Proceedings of 22nd European Conference on Modelling
and Simulation ECMS 2008, Nicosia, Cyprus, pp. 512-518, 2008.
[10] L. Macku, D. Samek, "Predictive control using neural network applied on
semi-batch reactor," in 18th International Conference on Process Control,
Tatranska Lomnica, Slovakia, June 1417, 2011.
[11] L. Macku, D. Samek, "Two step, PID and model predictive control applied
on fed batch process," in The 14th World Scientific and Engineering
Academy and Society (WSEAS) International Conference on Systems,
Latest Trends on Systems (Volume II), Corfu Island, Greece, pp. 470473,
July 22-24, 2010.
[12] Lanczos, "An iterative method for the solution of eigenvalue problem of
linear differential and integral operators," J. Res. Nat. Bur. Stand., pp. 255-
82, 1950.
[13] G. H. Golub, C. F. Van Loan, Matrix Computations, The Johns Hopkins
University Press, Baltimore and London, 1996, p. 470-507.
4
VII. BIOGRAPHIES
Seshu Kumar Damarla was born in Andhra Pradesh,
India on January 12, 1986. He got his B.Tech degree
from Bapatla Engineering College, Bapatla, Andhra
Pradesh, India. He completed his M.Tech from NIT
Rourkela, Orissa, India. Currently he is doing Ph.D in the
same institute. He is working on process identification,
monitoring and control.
Madhusree Kundu was born in Kolkata, 21 January
1965. She did her B.S.C. in Chemistry from university
of Calcutta, India. Dr. Kundu got her B.Tech and
M.Tech. in Chemical Engineering from the same
university in the years 1990 & 1992, respectively. She
completed her Doctoral study from Indian Institute of
Technology, Kaharagpur, India and was awarded
Ph.D. in the year 2005. She served as a Process
Engineer in the Simon carves India Ltd. during 1993-1998. She served as a
lecturer and then Assistant Professor in The Birla Institute of Technology &
Science, Pilani, India during 2004-2006. Presently, she is the Associate
Professor, Department of Chemical Engineering, NIT, Rourkela, Orissa, India.
She has published a couple of research articles and book chapters to her credit.
Fluid Phase Equilibria, Advanced Process Control, Process Monitoring & Fault
Detection and Diagnosis, are the current research interests of her. Dr. Kundu is
the life member of Indian Institute of Chemical Engineers (IIChE).
5