16th International Conference on Greenhouse Gas Control Technologies, GHGT-16

23rd -27th October 2022, Lyon, France

Multivariate data analysis of online-sensors and spectroscopic data

for the prediction of solvent composition parameters for MEA
Lars E. Williamsa, Audun Dragesetb*, Bjørn Grunga
University of Bergen, Department of Chemistry, Allégaten 41, 5020 Bergen, Norway
a
b
Technology Centre Mongstad (TCM), 5954 Mongstad, Norway

Abstract

Cost-effective operation of amine-based post-combustion CO2 capture facilities is important for successfully implementing the
technology on a broad industrial scale to reach current climate objectives. Technology Centre Mongstad has benchmarked
performance of such technologies in a generic amine plant since 2012. This work utilized historic plant process and laboratory data
collected during a test campaign with 2-aminoethan-1-ol (MEA) in 2015. The aim of this work was to employ multivariate analysis
to develop models to predict laboratory results for CO2 content (Total Inorganic Carbon) and amine functionalities (total alkalinity)
in the amine solvent. Predictive models were made based on process variables alone, spectroscopic data alone and data fusion
models. The process model could explain 99% of the variance for total inorganic carbon in the Lean solvent stream. The Rich
solvent is more chemically complex and requires the use of spectroscopic data to explain 95-99% of the variance. In this work we
demonstrated how multivariate data analysis can be employed to predict solvent parameters that can be reported in real time for
improved control of the capture process.

Keywords: MEA; Solvent monitring; Multivariate data analysis; post-combustion CO2 capture; Technology Centre Mongstad

1. Introduction

Decarbonizing heavy industries is a key for achieving the carbon mitigation goals outlined in the 6th report from the
Intergovernmental Panel on Climate Change (IPCC-6) [1]. Amine-based carbon capture is among the most mature
technologies for decarbonizing existing industrial point sources for CO2 emissions. Technology Centre Mongstad
(TCM) has operated and demonstrated generic and proprietary amine solvents for post-combustion carbon capture
(PCCC) since 2012 [2]. TCM is located on the west coast of Norway in the vicinity of Equinor’s oil refinery at
Mongstad. With access to two distinctly different industrial flue gases: combined-cycle gas turbine (CCGT)-based
combined-heat-and-power plant (CHP) and RFCC (Residual fluid catalytic cracker) and the ability to manipulate these
flue gases (through dilution and CO2 recycling), TCM can assess CO2 capture technologies under conditions that are
representative of multiple industries emissions [3]. Among the main objectives of TCM’s test campaigns are risk
reduction (economic and environmental) for commercial application and full-scale deployment of Carbon Capture
and Storage (CCS). Key among these test campaigns are the open test campaigns with non-proprietary solvents like
aqueous 2-aminoethan-1-ol (commonly known as Monoethanolamine or MEA) and the aqueous blend of 2-amino-2-

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 GHGT-16 Lars E. Williams 2

methylpropan-1-ol (AMP) and Piperazine (PZ). Data and learnings from these campaigns can be disseminated in line
with TCM’s purpose to ensure safe technology implementation to combat climate change.

Nomenclature

TCM Technology Centre Mongstad

CHP Combined heat and power gas turbine
MEA Monoethanolamine (2-aminoethan-1-ol)
TIC Total Inorganic Carbon
FTIR Fourier Transformed Infrared Spectroscopy
PCA Principal Component Analysis
PLS Partial Least Squares regression
MLR Multiple Linear Regression
Lean Refers to capture solvent stripped of CO2 to be used in absorption
Rich Refers to capture solvent rich in CO2 after absorption

MEA is a first-generation amine-based CO2 capture solvent. Amine based absorption is a reversible reaction between
an aqueous amine and an industrial flue gas containing CO2. The basic amine functionality reacts with CO2 to form a
carbamate, removing the CO2 from the gas and trapping it in the liquid phase. This reaction is carried out in the
absorber containing a packed gas-liquid contactor to ensure high mass transfer between the two phases at lower
temperatures (30 – 60 °C, depending on solvent and plant configuration). The reaction can then be reversed by
applying heat via a steam boiler in the stripper section (see Figure 1). CO2 is released as a product gas and the liquid
amine is regenerated and returned to the absorber. A capture plant operating with MEA can capture over 90% of the
CO2 (advanced solvents have demonstrated over 98% capture) and generates CO2 product with high purity (99.9%)
[3a]. The major challenge is the operational cost [4]. The capture plant should be operated under optimal conditions
to minimize energy consumption mainly tied to removing CO2 from the solvent. This is often reported as Specific
reboiler duty (SRD). To achieve this, operators are reliant on accurate gas composition data at the inlet and outlet of
the absorber as well as the solvent composition. Gas composition is monitored online (via gas chromatography or
infrared spectroscopy) and operators can quickly act on any changes in for example the CO2 concentration from the
industrial source. In contrast, the solvent composition is usually measured through extractive samples and laboratory
analysis, and results are only available after multiple hours and in some cases days.

This work utilized plant data from TCM’s MEA test campaign conducted in 2015 (July to October) funded by
Gassnova, Equinor (former Statoil), Shell and Sasol (TCM’s owners in that period). The campaign’s primary objective
was to conduct an updated baseline and plant performance with MEA and to verify plant mass balance over a set of
operational conditions, as well as other technology knowledge gaps [5]. The plant was operated with a 30 wt% aqueous
MEA solution and the CHP flue gas (3.6 vol% CO2) for most of the test period. Throughout the campaign laboratory
samples were collected and analysed to (a) ensure tests were conducted with correct amine concentration, (b) record
resulting lean loading (mole CO2 per mole of amine) during process optimization and (c) monitor solvent degradation
and plant corrosion.

The TCM amine plant has a large array of analytical instruments in the rich (CO2 rich solvent after absorption) and
lean (CO2 lean solvent after stripping solvent) streams. Among these are temperature, pH, conductivity, density, and
pressure, see Figure 1. The data is used for general purpose applications in characterising the physical parameters
during a test campaign. Such analytical instruments can potentially be used to predict solvent parameters currently
only available via laboratory analysis like (1) Total Inorganic Carbon (TIC); a measure of CO2 in the solvent, (2) Total
alkalinity (total NH functionality in the solvent as determined via an acid base titration) and (3) amine concentration.
These are used to calculate the CO2 loading of the solvent (mole CO2 per mole of amine). During the campaign Total
alkalinity was used as an analogue for amine concentration as the NH functionality is predominantly from MEA. It is
expected that predictive models would benefit from the addition of chemical information acquired through
spectroscopy, as spectroscopic methods like FTIR can give information about chemical bonds and functionality

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 GHGT-16 Lars E. Williams 3

present in the solvent. Such chemical information is necessary if the degradation [6] of the solvent and its impact on
the plant are to be monitored online [7].

In this paper we present how common online measurement principles like pH and conductivity can be used to predict
solvent parameters which were previously only obtained through laboratory analysis. In addition, the limitations of
this concept as well as how the addition of spectroscopy can improve the model accuracy is discussed. The
implementation of such models can improve plant efficiency and lower the frequency of sampling and analysis
resulting in a reduction of both exposure risks to operators and as well as costs for operating a laboratory.

Depleted Table 1. Process variables

F Flow metering flue gas Input variables Unit
C Composition Product CO2
M Online measurment Density kg/m3
S Sample location Conductivity µS/cm
Rich amine
pH
C

Temperature °C
Density kg/m3
Water Conductivity µS/cm
Washes Lean amine
pH
Temperature °C
CHP Inlet flue gas m3/h
Stripper Inlet CO2 %
Steam
Absorber Absorber Outlet CO2 %
M S
M Sump level mm
Lean solvent kg/h
Flue gas
Inlet
C F Condensate Rich solvent kg/h
M M S
Liquid Temp. °C
Stripper
Pressure barg
Liquid level mm
Atmospheric pressure bar
Conductivity Density Pressure Temperature
(µS/cm) (kg/m3)
pH
(mBar) (°C) Output variables Unit
TIC mol/kg
Rich
Lean solvent and stripper online data Tot.Alk mol/kg
TIC mol/kg
Lean
Tot.Alk mol/kg
IR
Conductivity Density
CO2 pH
(µS/cm) (kg/m3)
(vol%)

Rich solvent and absorber online data

Figure 1. Simplified process flow diagram of TCM amine plant with CHP flue gas
configuration. The Flue gas is introduced to the bottom of the absorber column
where it is brought into contact with MEA solvent in a counter current gas
absorption process in the yellow packing section. The CO2 rich solvent is sent for
regeneration in the stripper where CO2 is released, the CO2 lean solvent is returned
to the absorber column. Some online measurement points and variables used in this
work are highlighted

1.1. Latent variable modelling

Latent variables are linear combinations of the measured variables. They represent excellent tools for data
visualization and quantitative modelling. Two main types of latent variable analysis have been used in this work.
Principal Component Analysis (PCA) [8] and Partial Least Squares Regression (PLS) [9].

Any data set not based on an orthogonal design will have correlations among the variables. This makes it possible
to go from a large number of measured variables to a much smaller number of latent variables while preserving the
information content of the data. This concept is particularly useful for data exploration but can also be used in
classification and regression analysis. In PCA, latent variables are referred to as principal components. These are

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 GHGT-16 Lars E. Williams 4

constructed so that they capture as much of the variance in the data as possible. This is known as the maximum
variance criterion. Each measured variable contributes to each latent variable, but the amount of contribution is
different for different variables. Each measured object has a score on each latent variable, just like every object has a
value for the measured variables. The collection of scores on a latent variable is referred to as a score vector, and a
bivariate scatter plot of the first two score vectors after PCA is the two-dimensional plot that explains as much variation
as possible. For this reason, PCA is extremely popular for data exploration, and it is used in a variety of scientific
fields, although under different names.

All data contains noise. This fact means that the usefulness of principal components extends beyond data
exploration. They can be used in classification and discrimination analysis, and regression. This can be done by
calculating enough principal components to capture the systematic variation in the data. Using these principal
components in further analysis and ignoring the residual variation left unmodelled ensures that noise in the data does
not pollute the quality of the subsequent models. In this aspect, PCA can be seen as a denoising technique.

In this work, principal components have been used for data fusion [10], which is the term used for uniting different
sets of data into one data set. The present work deals with traditional process data and infrared spectra used to
characterize the state of an amine solution used to absorb CO2. It is tempting to combine these two measurement types
to better describe the system’s state. Doing so, one immediately finds that the number of relevant spectral variables is
significantly larger than the number of process variables. Simply fusing the two sets of measurements by adding one
set of variables to the other will lead to a data matrix completely dominated by the spectral data. Deleting spectral
variables so that the two sets become equal in size is another strategy, but there is a risk of throwing away useful
information.

Furthermore, making a proper variable selection is not trivial. In this work, PCA is done on the spectral data. The
number of principal components calculated and retained is enough to capture the systematic variation of the data. This
number is independent of the number of variables in the data set but is decided by the number of independent sources
of variation in the data. In this way one can reduce thousands of measured variables to a handful of principal
components without any information loss. As the spectral variables are very correlated the reduction is substantial.
This means the process data is joined with the significant score vectors from a PCA, not the measured spectral
variables.

Principal components can also be used in regression analysis. This is referred to as Principal Component Regression
(PCR). In multiple linear regression (MLR), one would model a response (e.g., total alkalinity of a solution) as a
function of a set of measured variables, such as the process variables used in this work. There are many problems with
this approach. In MLR it is assumed that the error in the independent variables is much less than the error in the
response. This is not necessarily the case, and if this is violated the MLR model is not the optimal model. A further
complication is that the regressors are assumed to be independent variables – they should be independent of each
other. If they are not, neither the model predictions nor the interpretation of the effects of the regressors (the regression
coefficients) may be trusted. Moving from a set of highly collinear measured variables to a set of orthogonal latent
variables and using these as regressors elegantly avoids this problem. A further benefit of this approach is that the
principal components are much less influenced by noise than the original data set. Where MLR uses all the data
available, a latent variable regression model using principal components would only use the systematic part of the
data as regressors.

While PCR in most cases is favourable to MLR, it is still not the preferred latent variable regression technique. The
problem with the principal components is that they are constructed to capture all the main sources of systematic
behaviour. Not all these systematic sources of variation will be relevant to the regression problem. A simple example
would be the prediction of the concentration of a compound in a sample using spectroscopy. While changes in the
analyte concentration surely impacts the spectra, so will any changes in the concentrations of other compounds present
in the sample. This is systematic behaviour that will be picked up by the principal components, but it is not relevant
for the prediction of our analyte. PLS is the solution to this problem.

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In PLS the latent variables are calculated differently from the ones in PCA. Instead of focusing on the variance of
the independent variables, PLS uses the covariance between the independent variables and the response as the latent
variables. This means that the latent variables are directly related to the response modelled. Where PCR asks the
question “what are the major sources of variation in my data?”, PLS asks “what part of my data varies in the same
way as the response?”. This makes PLS a more powerful regression technique than PCR. They are both latent variable
regression techniques, but the latent variables used in the regression are quite different.

2. Experimental section

The TCM amine plant is a generic plant designed and built by Aker Solutions and Kværner with a capacity to treat up
to 60 000 Sm3/h post combustion flue gas. The plant was operated with the Combined Heat and Power flue gas with
a CO2 concentration of 3.6 % and aqueous MEA (30 wt%). The absorber tower was operated with an 18- and 24-
meter packing section and a lean amine flow of 43 000 – 70 000 kg/h. The stripper section was operated at 120.0 –
121.5 °C. Detailed plant parameters for different test phases are described in the literature [5]. Solvent parameters
were monitored via in-line liquid conductivity (Endress Hauser, resistance measurement conductivity meter), density
(Coriolis mass flow, Proline Promass 80F) and pH meter (Endress Hauser, potentiometric pH measurement) installed
after circulation pumps on rich and lean solvent flow (see Table 1). The process data are measured at different time
intervals. In this work, values averaged over a period of 15 minutes were used for all variables.

The process data needs to be cleaned up prior to further analysis as the measurements are carried out continuously,
regardless of the system state. Measurements taken during outlying conditions were removed from the data sets.
Examples of outlying conditions are system shutdown periods, the recovery phase after such shutdowns and periods
of MEA reclamation.

Extractive liquid samples were collected via a fast loop system equipped with a process sampler (DOPAK Inc.) by
operators on a regular basis and delivered to TCM onsite laboratory for storage and further analysis.

Rich and lean liquid samples were analysed with a Bruker Alpha FTIR Spectrometer with a diamond ATR cell (Bruker
Corporation). Spectra were recorded between ~4000 and ~425 cm-1. A plot of the raw spectra (Figure 2) shows that
there is no relevant information above 3640 cm-1 or below 800 cm-1. The same applies to the region between 2750 cm-
1
and 1730 cm-1. These regions were removed from the spectra prior to further analysis.

The number of samples used in the models varies for the different responses and type of data. The analytical laboratory
did not measure all responses for all samples, and IR spectra were not recorded for all samples. Table 2 shows the
number of samples used in each model.

Table 2. Model development

Variable name Type data Number of objects
Lean Online 101
TIC Spectra 52
Rich
Online and spectra 52
Online 52
Tot.Alk Rich
Spectra 48

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 GHGT-16 Lars E. Williams 6

Figure 2. FTIR spectra of rich solvent samples.

Total Alkalinity is analysed via automated acid base titration with HCl (1.0 M). The reported uncertainty is 2%. Total
Inorganic Carbon (TIC) is analysed with a TOC/TN Elementar (Elementar Analysensysteme GmbH). The reported
uncertainty is 4%.

3. Results and discussion

4.1 Prediction of properties using only process data

4.1.1 Lean TIC predicted from process data

As the process data is a mix of variables expressed using different measurement units, the data was standardized and
mean centred prior to modelling. An initial PLS regression of the process data with the lean TIC as a response yielded
an 8-component model explaining more than 98 % of the variance in the TIC. The number of components was
determined using cross validation [11]. This is more than satisfactory as the uncertainty in the laboratory
measurements is approximately 4 %.

Not all recorded variables contribute to the regression models. Since the presence of irrelevant predictors may be of
detriment to the model, care was taken to remove any predictor variables with a small regression coefficient and a
large uncertainty. This also leads to a simpler model – one with fewer PLS components. The final Lean TIC model
contained six PLS components and captured 99 % of the variance of the response. Figure 3 shows the regression
coefficients of the variables in the final model.

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 GHGT-16 Lars E. Williams 7

1.2000

1.0000

Weighted Reg. Coeff (TIC Lean)

0.8000

0.6000

0.4000

0.2000

0.0000

-0.2000

-0.4000
Ric Ric Ric Ric Lea L Lea Str
h Den h Co hp hT n D ean C np ip p
er V
sity ndu H em ens ond H
ctiv per it y u ct .pr e
ity a ture ivit ssu
y re
Variables

Figure 3. Bar plot of the regression coefficients in the final Lean TIC model.

1.8000

1.6000

1.4000
TIC Lean

1.2000

1.0000

0.8000

0.6000
19 27 34 39 44 49 55 60 65 72 79 84 89 96 102 107 112 117 122 127 133
Objects

Figure 4. Actual (blue) and predicted (red) Lean TIC values for the final model.

4.1.2 Rich Total alkalinity predicted from the process data

The enriched amine solution resulting from the CO2 capture is more complex chemically. Various chemical reactions
take place in the mixture, and it is expected that a model based on the process data alone will struggle to explain the
behaviour of the solution.

Figure 4 shows the poor performance of an optimized (irrelevant variables removed) PLS model of the Rich Total
Alkalinity value. The two-component model only explains 52.81 % of the response. This demonstrates that while the
process variables may be enough to satisfactorily model the simpler lean system, more information is needed to obtain
acceptable models for the more complex rich flow.

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5.1 Pred
Raw
5

4.9

Tot Alk Rich

4.8

4.7

4.6

4.5

4.4
19 23 29 32 36 41 43 53 58 62 66 70 76 80 84 88 93 102 106 110113 116 120123 127 130
Objects

Figure 5. Actual (blue) and predicted (red) total alkalinity in the rich solvent.

4.2 Predictions from IR spectra

As shown in 4.1.2, process data alone is not sufficient for prediction of many of the properties. Infrared spectra
represent an alternative information source. An infrared spectrum contains information on the functional groups and
chemical bonds present in a sample. Figure 6 shows two spectra: One from a lean sample and one from a rich sample.
It is evident that the two samples have strong similarities, but also that there are differences.

Figure 6. Spectra of a lean (blue) and rich (red) mixture.

The models presented in this section use whole spectral profiles (from the regions described in the Experimental
section) as predictor variables. This necessitates different pre-treatment compared to the process data. Standardization
is not an appropriate tool for profile data, as that would inflate small, noisy variables and reduce the contribution from
the larger, more interesting variables. The effects that usually cause problems when using spectral profiles as
predictors are additive baseline effects and multiplicative effects due to light scattering. In this work, the baseline
effects were handled by Savitzky-Golay second order differentiation [12] with a window size of 25 and a cubic
polynomial. The multiplicative effects were handled by Extended Multiplicative Scatter Correction [13].

4.2.1 Rich Total Alkalinity modelled from IR spectra

Figure 7 shows the performance of a three component PLS model for predicting the total alkalinity in the rich samples.
For this model, the Total Alkalinity values were root transformed. This improves the model quality. The model
captures 95.56 % of the variance of the data and compared to the model shown in Figure 5 the IR model improves the
performance to a remarkable extent.

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5.1 Pred
Raw
5

Rich Tot Alk 4.9

4.8

4.7

4.6

4.5

4.4
1 9 12 19 30 33 37 43 45 55 62 66 83 86 91 97 110 113 116 119 125 128 132 137
Objects

Figure 7. Performance of a three component PLS model of the IR spectra. The actual
Total Alkalinity is shown in blue, and the predicted values in red.

4.2.2. Rich TIC modelled from IR spectra

Although not shown in this work, attempts were made to model the TIC of the rich solvent using only the online
process data. The resulting model was only able to explain 59.46 % of the response variance. It is therefore interesting
to see if the performance improves when replacing the process data with the IR spectra. The best model of the IR data
explained 81.66 % of the response. While this is an improvement, Figure 8 shows that there is still room for
improvement. The next logical thing to try is then a combination of the process and IR data.
2.55 Pred
Raw
2.5

2.45

2.4
Rich TIC

2.35

2.3

2.25

2.2

2.15
20 24 31 33 42 44 49 58 62 66 71 76 84 88 93 98 106 110 116 119 121 125 127 129 131
Objects

Figure 8. Performance of a two component PLS model of the IR spectra. The actual
TIC is shown in blue, and the predicted values in red.

4.3 Combining process data and IR spectra: Data fusion model of the rich TIC
An immediate challenge presents itself when trying to combine the online process data and the IR spectra. The number
of spectral variables is more than 250 times larger than the process variables. This means that a simple fusion where
the spectra are simply added to the process variables will lead to a data matrix completely dominated by the spectral
information. More advanced fusion methods are therefore needed.

In this work, the spectral data was decomposed using Principal Component Analysis. Enough components were
extracted to explain 99 % of the variance of the spectra. The number of components, which typically is quite small,
was found using cross validation. The corresponding significant score vectors were subsequently appended to the
process data, resulting in new variables.

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Three principal components were enough to reach more than 99 % variance explained for the spectra used in the
modelling of the rich TIC. The resulting model was able to explain 87 % of the variance of the response. The
performance is illustrated in Figure 9. While far from perfect, it is still the best model variable, and is good enough to
predict the general variations in the response.

2.6 Pred
Raw

2.5

2.4
TIC Rich

2.3

2.2

2.1
19 21 30 32 40 42 47 58 62 66 70 79 82 86 92 101 105 111 114 116 120 122 124 127 132 134
Objects
Figure 9. Performance of a ten component PLS model of the IR spectra. The actual
TIC is shown in blue, and the predicted values in red.

While the model still has problems with picking up the finer changes in the response, it is clear that the combination
of process and IR data has improved the performance.

4. Conclusion

This work has demonstrated the possibility of predicting relevant parameters describing the state of a MEA solvent
used in CO2 capture. For some responses, solid models are achieved only using online process measurements. More
complex situations benefit from the usage of IR spectra. The best models are achieved by combining both sets of data
using data fusion techniques.

This work has been carried out on historical data from a campaign several years old. This represents challenges, as
the detection and exclusion of outlying conditions becomes more difficult. A model is never better than the data from
which it was created, so cleaning the data from outlying conditions is important.

This work demonstrates how multivariate models from process and spectral data can be used to predict the state of
the solvent mixture and the efficiency of the capturing process. It is paramount that the sample set from which the
model is created is representative for all the states the system may occupy in the future. Samples from both fresh and
various degrees of degraded solvent states must be used. This should not represent a problem for a plant operating
under relatively constant conditions.

Continuous monitoring of plant conditions is vital for cost-effective plant operation. This includes the monitoring of
solvent conditions both in the lean and the rich stream. Laboratory analyses contribute to the operational expenses
(OPEX) of the capture plant and a significant reduction in the scope of laboratory analysis can be a major cost saving
for a full-scale plant. In addition, models can be incorporated into the control system so operators can take immediate
action to keep the plant running optimally. As this work demonstrates, models can accurately predict standard
laboratory parameters and can improve response time to changes in the plant. This work illustrate how technology
developers can utilize process measurements and spectroscopy to improve the control of the plant. The method is not
solvent or plant specific and can be used in screening historic datasets to guide further technology development.

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5. Acknowledgment

The authors gratefully acknowledge the staff of TCM DA, Gassnova, Equinor, Shell and TotalEnergies for their
contribution and work at the TCM DA facility. The authors also gratefully acknowledge Gassnova, Equinor, Shell,
and TotalEnergies as the owners of TCM DA for their financial support and contributions.

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