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Analysis of TRS emissions from recovery boilers

ENZO M. E. P. REYES1, LEONARDO C. DE OLIVEIRA2, DANIEL M. SATURNINO3, ESA
VAKKILAINEN4 AND MARCELO CARDOSO5
1
Superintendent of Black Liquor Recovery Area
Celulosa Arauco y Constitución S.A.
Planta Valdivia, Chile.
2
Masters student 3 Post-doctorate Student
Dept. Chemical Engineering
Federal University of Minas Gerais
UFMG, Belo Horizonte, MG, Brazil.
4
Professor
Dept. of Energy and Environmental Technology
Faculty of Technology
Lappeenranta University of Technology, Lappeenranta, Finland.
5
Professor and corresponding author (mcardoso@deq.ufmg.br)
Dept. Chemical Engineering
Federal University of Minas Gerais – UFMG
Zip Code 31.270-901, Belo Horizonte/MG, Brazil.

SUMMARY
This paper analyses the influence of operating variables on flue gas emissions containing total reduced sulfur (TRS) from
a dissolving tank and a recovery boiler. Two pulp mills in Chile provided data to allow this study to be conducted. First,
at Lincacel plant, emissions from the dissolving tank vent gas scrubber were studied. Then at the Valdivia plant, the
influence of different operating variables on TRS emissions from the recovery boiler were analysed using a multivariate
statistical analysis for TRS emissions. In this analysis it was observed that variables affecting the boiler furnace
temperature were strongly correlated with changes in the TRS emissions.

INTRODUCTION
As technology advances, newer equipment in the chemical
recovery area is allowing operation with low TRS emissions.
However, older mills close to urban centres still face problems
with odorous emissions (1). In Kraft pulp mills, odour is caused
mainly by reduced sulfur compounds (total reduced sulfur -
TRS): methyl mercaptan (MM) - CH3SCH, dimethyl sulfide
(DMS) - CH3SCH3, dimethyl disulfide (DMDS) - CH3S2CH3
and hydrogen sulfide - H2S. MM, DMS, DMDS and H2S are
formed in the pulping process of wood; while SO2 and H2S are
mainly formed in the recovery boiler (2). TRS combined with
air and water, plus varying amounts of vaporous methanol and
turpentine, are collectively known as non-condensable gases
(NCG). NCG originates in many areas of the mill. There are
basically two types of NCG: concentrated NCG (CNCG) and
diluted NCG (DNCG) (3).
There are two approaches to reducing odours: one involves the
elimination of TRS by thermal oxidation, usually performed
through combustion of NCG and DNCG in lime kilns, power
boilers, recovery boilers or dedicated incinerators. The other
approach is to use vent gas scrubbers, where diluted gases MM,
H2S and other NCG are contacted with water and / or white
liquor sprayed on the washers.
Although vent scrubbers are very effective in removing NCG
from the gas streams, some do not achieve the expected
performance. In this study, the scrubbers installed at the
dissolving tank connected to a recovery boiler presented such
problem. The dissolving tank receives the smelt drained from
the base of the recovery boiler which contains mainly sodium
sulfide and sodium carbonate. The smelt droplets are dissolved
in weak white liquor to produce green liquor. To avoid explosions
in the dissolving tank during the dissolution process, steam jets
are used to break the flow of smelt coming out of the boiler
before it reaches the white liquor (4). This steam atomization,
which pulverizes the smelt into small droplets, together with the
smelt dissolution generates gases in the dissolving tank.
This paper has two objectives: to identify the sources of TRS
emissions from the dissolving tank vent gas scrubbers in the
Lincacel plant and to evaluate the impact of boiler operating
conditions on the TRS emissions from the recovery boiler at the
Valdivia plant, both located in Chile.
STUDY BACKGROUND
Chilean Supreme Decree, number 167 of 1999, from the
Secretary General of the Presidency of the Republic of Chile
regulates the level of TRS emissions from the recovery boiler’s
dissolving tank. This standard decrees that it is inappropriate if
5% of the TRS values measured per year are greater than 16.8 mg
H2S / kg DS. A control measurement of TRS emissions from the
dissolving tank should be carried out at least once annually. This
standard also decrees that in the combustion of black liquor in the
recovery boiler, TRS in the flue gas should not exceed 5 ppmv,
measured on a dry basis and corrected to 8% oxygen (5).
In the period of 2008 to 2009, a series of TRS measurements in
the dissolving tank were made at the Lincacel plant. Some of
the values were above 16.8 milligrams of H2S per kilogram of
dry solids and these values led to an investigation to determine

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changes in the operating variables of the dissolving tank. High
values were also the motivating factor for having an analysis of
TRS emissions done in the recovery boiler at Valdivia plant (5).
The dissolving tank system and the recovery boiler at Lincacel
plant were built in 1993.The scrubber has four shower heads
placed in a specific arrangement at the same height from which
the weak white liquor or water is sprayed. Each shower head
contains a series of nozzles that atomizes water or weak white
liquor through a circulation pump. The dissolving tank from this
plant can also receive streams from other stages of the process
containing contaminated condensate that can come from the
evaporation, causticizing and the pulping systems.
The recovery boiler at Valdivia plant was built in 2003. The
boiler is designed to burn 3,100 tons of dry solids per day,
producing 457 tons per hour of steam at a pressure of 86 bars
and temperature of 486 °C. In this boiler there is the possibility
of burning alternative fuels as well as fuel oil. In addition,
the boiler burns methanol and non-condensable gases from
the digesters and evaporators.
TRS EMISSIONS
The main sources of TRS emissions from the chimneys of the
dissolving tank can be divided into three main categories: (i)
TRS emissions from green liquor and weak wash, (ii) emissions
of H2S from the smelt atomization with steam jets, and (iii)
emissions of methyl mercaptan (6). According to Frederick et
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al (7) and Danko (8) the largest emissions of H2S comes from
green and white liquors. Also, the causticity has less influence
on the emissions of TRS than sulfidity. The emissions of H 2S
from the smelt atomization with steam usually occur from the
reactions of sodium sulfide (Na2S) smelt with water vapour and
CO2, through the reactions [1] and [2]:
Na2S + 2 H22ļ+2S(g) + 2 NaOH [1]
Na2S + H2O + CO2ļ+2S(g) + Na2CO3 [2]
Their results showed that at a low partial pressure of O2, the
partial pressure of H2S depends on the partial pressure of water
vapour and CO2. For a partial pressure of CO2 in the flue gas of
0.4% and low oxygen concentrations, the concentration of H 2S
at equilibrium was calculated to be approximately 700 ppm at
1000 K and less for the temperatures lower than 1000 K.
Another important category to be analysed is the emissions
of organic sulfur compounds such as MM and DMS which
can enter the dissolving tank through the condensate from
the causticizing and evaporation areas. The condensate from
evaporation usually contains methanol (CH3OH) and this can be
found in emissions from the dissolving tank as well. Kymäläinen
et al. (9) found emissions at concentrations of 50 ppm in the
dissolving tank. In addition, methanol often reacts with H 2S in
the gas phase to produce MM. According to Ziolek et al. (10),
the alkaline environment that favours this reaction is typically
catalysed by sodium and carbonate ions.
In boiler emissions, the main controlling factor in vaporization
of compounds containing sulfur and sodium is the temperature
in the furnace. According to Hupa (11), the concentration of
sodium-containing compounds in the gas phase increases with
increasing temperature, while emission of sulfur-containing
compounds decrease with temperature increase.
Besides temperature, the ratio of the concentrations of sulfur and
sodium in the black liquor will also influence the composition
of compounds containing sulfur and sodium present in the gas
stream. The average molar ratio of sulfur to sodium can vary
in the range from 0.8 to 1.5 in the recovery boiler combustion
gases. This ratio is lower at higher furnace temperature.
As the gases rise to the top of the furnace and combustion is
completed, several chemical reactions occur leading to the
formation of recovery boiler ashes. As a result, the boiler flue
gas composition is affected in different ways. In the case of
a hot bed in the bottom of the boiler, ash production is larger
Fig. 1. Schematic Diagram of Recovery Boiler at
Valdivia mill. The numbers on the Figure refer to
measurement described in Table 1.
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with increased formation of carbonate and sodium sulfate and
consequently a greater reduction of TRS emissions. On the
other hand, in the case of a cold bed, less ash production occurs
and there is an increase in TRS emissions in the flue gas.
METHODOLOGY
DISSOLVING TANK MEASUREMENTS AT
LINCACEL PLANT
During 2008 and 2009 a series of measurements of TRS
concentration in the gases entering and exiting the dissolving
tank scrubber were made. The evaluations took place during
normal operating conditions with the dissolving tank using
weak liquor to wash the gas and also periods with changes in the
operating conditions of the boiler and washing media.
Periodic maintenance and other changes were carried out in the
dissolving tank / scrubber system during this period, including:
Table 1. Variables considered in the analysis of the Valdivia mill
(i) cleaning of all the scrubber shower nozzles, (ii) changing
the exhaust system by altering the fan speed and lock system
to prevent entry of air into the scrubber, (iii) increasing the
reflux of white liquor or water in the system through the pump
recirculation, (iv) replacing the white liquor with an alkaline
aqueous solution with pH 13 (NaOH added to water), and
(v) checking for and removing any possible input of gas and
condensate containing sulfur compounds in the dissolving tank
scrubber that could come from others areas of the pulp mill.
RECOVERY BOILER STUDY AT VALDIVIA
PLANT
During 2010 a set of data was collected and divided into three
periods: the first corresponds to the entire year of 2010 with
data points consisting of hourly averages (total of 1117 data sets
including the analysis of white liquor sulfidity performed in
the laboratory). The second set covers the entire month of June
2010, and the third set only covers the last 53 hours and ten

Var. Description Unit Var. Description Unit

1 Time Days 38 Inlet gas temperature in dissolving tank scrubber °C

2 Primary air flow Nm3/s 39 Gas pressure in the DNCG collector kPa
3 Temperature of primary air °C 40 Temperature of DNCG gas °C
4 Pressure of primary air that enters the boiler kPa 41 Flow of the DNCG gases that enter with the secondary air Nm3/s
5 Pressure of the primary air kPa 42 Temperature of the DNCG gases that enter with the secondary air °C
6 Lower secondary air flow Nm3/s 43 Pressure of the secondary air when the DNCG gases enter at point 1 kPa
7 Lower secondary air temperature °C 44 Pressure of the secondary air when the DNCG gases enter at point 2 kPa
8 Pressure of lower secondary air kPa 45 NCG gas flow in the boiler Nm3/s
9 Pressure of lower secondary air that enters the boiler kPa 46 Pressure of entering NCG gases kPa
10 Air flow upper secondary Nm3/s 47 Temperature of entering NCG gases °C
11 Upper secondary air temperature °C 48 Flow of methanol into the burner kg/s
12 Pressure at the secondary air inlet of boiler kPa 49 Pressure of methanol in the burner kPa
13 Pressure at the top secondary air inlet of boiler kPa 50 Pressure of methanol in the burner 2 kPa
14 Tertiary air flow Nm3/s 51 Oil flow in the NCG burners kg/s
15 Tertiary air temperature °C 52 Oil pressure in the NCG burners kPa
16 Pressure of tertiary air that enters the boiler 1 kPa 53 Oil flow in the burners kPa
17 Pressure of tertiary air that enters the boiler 2 kPa 54 Oil pressure in the burners MPa
18 Gas flow in dissolving tank Nm3/s 55 Oil flow in the burner 2 kg/s
19 Gas pressure in dissolving tank kPa 56 Oil pressure in the burner 2 MPa
20 Gas flow in mixing tank Nm3/s 57 Differential pressure of the upper side of boiler bank kg/s
21 Gas pressure in mixing tank kPa 58 Temperature of the upper side of boiler bank °C
22 DNCG gas flow in the boiler Nm3/s 59 Differential pressure of the underside of boiler bank kPa
23 Black liquor input stream in the boiler l/s 60 Temperature of the underside of boiler bank °C
24 Temperature of black liquor when entering the boiler °C 61 Difference of pressure at the top side of the economizer 2 kPa
25 Pressure of black liquor entering the boiler MPa 62 Temperature at the top of the economizer 2 °C
26 % of black liquor solids % 63 Difference of pressure at the bottom of the economizer 2 kPa
27 Pressure of liquor inlet , back wall MPa 64 Temperature at the bottom of the economizer 2 °C
28 Pressure of liquor inlet, left wall MPa 65 Difference of pressure at the top of the economizer 1 kPa
29 Pressure of liquor inlet , front wall MPa 66 Temperature at the top of the economizer 1 °C
30 Pressure of liquor inlet , right wall MPa 67 Difference of pressure at the bottom of the economizer 1 kPa
31 Temperature at point 1 inside the furnace °C 68 Temperature at the bottom of the economizer 1 °C
32 Temperature at point 2 inside the furnace °C 69 Pressure in the boiler furnace kPa
33 Black liquor reflux l/s 70 Oxygen content at point 1 %
34 Outlet pressure of the gases in dissolving tank kPa 71 Oxygen content at point 2 %
35 Outlet temperature of the gases in dissolving tank °C 72 Rate of dry solids incinerated Kg/S
36 Pressure in dissolving-tank scrubber kPa 73 White liquor sulfidity %
37 Outlet gas temperature in dissolving tank scrubber °C 74 TRS ppm

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minutes of June 2010. For the last two categories the data was
extracted at intervals of 5 minutes from the DSC (Distributed
Control System). After the removal of inconsistent data, a
study was conducted to find possible correlations among the 72
operational variables (Fig 1 and Table 1) and the TRS emission.
The Inferator program, developed by Oliveira (12) using Matlab
at the Federal University of Minas Gerais, was used to analyse
the operational variables that influence the emissions of TRS
in the recovery boiler of Valdivia plant. This program uses
multivariate linear regression techniques including principal
components regression, partial least squares, neural networks
with multi-layers perception type, and radial basis to evaluate
the datasets fed into the program.
Initially, the data was extracted from the DCS and stored in
Fig. 3. TRS Emissions during Black Liquor Gun Replacement.
Microsoft Office Excel worksheets. The data was first collected
Dashed line indicates regulatory limit.
on 72 variables, (Table 1), in order to correlate these variables
with the TRS emissions from the boiler. Data of TRS emissions
with negative values that represents a failure of the measurement
system were eliminated. The Hampel identifier technique was
also used to detect and eliminate outliers.
Based on Pearson correlation coefficients R 2 and stepwise
regressions, the influence of each variable was quantified.
From this analysis, regression variables of each set of system
data were obtained to establish which variables had a key role
in TRS emissions in the categories of data evaluated. From
these regression variables, neural network models were built
in order to predict TRS emissions. Two models were tested -
neural multilayer perceptions and radial basis -, for each data set
evaluated. A general scheme of the recovery boiler at Valdivia
plant indicates some of the points where the values were Fig. 4. TRS Emissions during Black Liquor Gun Shutdown.
measured (Fig. 1). Dashed line indicates the regulatory limit

RESULTS AND DISCUSSION
DISSOLVING TANK MEASUREMENTS AT
LINCACEL PLANT
The initial control steps taken in the Lincacel plant were
primarily based on literature studies which focused on the
reduction of the amount of H2S released in the dissolving tank.
The literature suggested that reduction could be achieved by
lowering the gases vent and steam pressure at the shatter jets
and by using more efficient nozzles in the scrubber.
However, the measurements done during the period of 2008 and
2009 indicated that these changes had had little or no effect.
After rigorously surveying the dissolving tank inlet and outlet
streams, and carrying out a careful mass balance, it was found
that the sulfur-containing compounds and methanol were
entering the dissolving tank through contaminated condensate
used to produce the green and weak white liquor. Up to that point,
the changes in the scrubber washing media had not involved the
removal of the condensates coming from the evaporation plant.
Only when these condensates were removed, was there a
significant reduction in emission levels of TRS. Emissions that
were previously superior to 8.16 mg H2S / kg DS fell to levels in
the range from 2.8 to 4.5 mg H2S / kg DS. Because of this, it was
decided not to reuse the contaminated condensates as washing
media in the dissolving tank scrubbers.

RECOVERY BOILER STUDY AT VALDIVIA

Fig. 2. TRS Emission Events for the Month of June 2010.
Dashed line indicates regulatory limit.
PLANT
DATA ANALYSIS
Data from the month of June was chosen because major
fluctuations in emissions of TRS occurred that month.
Observing the data after the removal of inconsistent points,
three events with TRS emissions higher than 1 ppmv can be
observed (Fig. 2). The remainder of the month shows the boiler
under stable operating conditions. For illustration purposes the
regulatory limit is also seen in Figure 2.
In order to better understand these events, the boiler historical
log was checked. The first event was connected with problems
in the black liquor guns, which affected the black liquor droplet
size and led to fluctuations in the boiler operating conditions.
As seen in Figure 3, the TRS emissions increased temporarily

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Fig. 5. Variables affecting the TRS emissions for the dataset of
2010.
Fig. 6. Prediction of TRS emission by best neural network model
for the dataset of 2010.
Fig. 7. Variables affecting the TRS emissions for the dataset of
June 2010.
and the problem was solved after some black liquor guns were
replaced. The second event was related to a trip problem in the
black liquor feeding pumps electrical circuit, what resulted in
a shutdown of liquor input to the boiler. Auxiliary burners and
start-up burners were put into service until the problem was
fixed. TRS emissions during this period increased significantly
as shown in Figure 4. Finally, the third event involved a
calibration of the TRS monitoring equipment, apparently not
relating to real boiler emissions.
RECOVERY BOILER EMISSION MODELLING
After the main operating variable data of the recovery boiler
were collected, a databank covering the entire year of 2010
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was built. The influence of these variables on TRS emissions
was evaluated using the R 2 coefficient based on the analysis of
Pearson correlation as shown in Figure 5. It can be observed
that the greatest effect on emissions during this period was the
furnace temperature, which was measured by thermographic
cameras. The second greatest effect was the inlet temperature of
non-condensable gases diluted in the secondary air.
Figure 5 also shows the variables selected for the development
of the regression and the neural network model. In total, 13
regression variables were obtained. The variables with higher
correlations and therefore more influence on TRS emissions
are: furnace temperature; inlet temperature of DNCG gas; oil
pressure in the burners; oxygen at point 2; pressure in the boiler
furnace; temperature of primary air; outlet pressure of the gases
in dissolving tank; pressure of tertiary air that enters the boiler;
oil flow in the burners; temperature of the upper side of boiler
bank; gas pressure in the DNCG collector; differential pressure
of the underside of boiler bank and upper secondary air flow.
We obtained a neural network model of Back Propagation type
with a hidden layer with four neurons which generated values
that showed a correlation equal to 0.74 and a mean absolute error
0.26 ppmv as shown in Figure 6.
In the second time period, regarding the month of June 2010, a
total of 8639 data sets were extracted. After the filtering step there
remained 8082 data sets, corresponding to 93.5% of collected data.
After the collection of the boiler variables covering the month of
June 2010, the R2 coefficients were obtained based on the analysis
of Pearson correlation to identify the variables that influence the
TRS emissions for this dataset (Fig. 7).
It may be also noted that for this period, the variables with greatest
influence on TRS emissions were associated with temperatures and
Fig. 8. Prediction of TRS emission by best neural network model for
the dataset of June 2010
flows of primary and secondary air, temperature and flow of non-
condensable gases, black liquor dry solids, oxygen content, and
white liquor sulfidity. However these variables are not the same as
those that were important for the data covering the entire year of
2010. This possibly occurred because of the impact of the transient
events showed in Figures 2 to 4 that affected the influence of the
variables during this short period of time.
In total for June 2010, 24 regression variables that influence TRS
emissions were found, which corresponded to 33% of the total
input variables. The variables that have higher correlations and
therefore more influence on TRS emissions are: primary air flow;
temperature of primary air; air pressure in the primary entrance
to boiler; lower secondary air temperature; upper secondary air
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flow; upper secondary air temperature; tertiary air flow; gas flow in
dissolving tank; outlet pressure of the gases in dissolving tank; outlet
temperature of the gases in dissolving tank; outlet gas temperature
in dissolving tank scrubber; inlet gas temperature in dissolving tank
scrubber; flow of the DNCG gases that enter with the secondary
air; temperature of the DNCG gases that enter with the secondary
air; NCG gas flow in the boiler; temperature entering NCG gases;
pressure of methanol in the methanol burner; oil flow in the burners;
temperature of the underside of boiler bank; difference of pressure at
the bottom of the economizer 2; oxygen content at point 1; rate of dry
solids incinerated and white liquor sulfidity.
The best neural network model obtained for the month of June 2010
used the Bayesian regularization with a hidden layer of four neurons,
and showed a correlation equal to 0.47 and a mean absolute error
Table 2. Three variables selected for the development of neural
model for the end of June 2010.
Variable Description Unit
40 Flow of the DNCG gases that enter with the secondary air Nm3/s
47 Flow of methanol into the methanol burner Kg/s
49 Pressure of methanol in the methanol burner 2 kPa
Fig. 9. Variables affecting the TRS emissions for the dataset of the
last 53 hours and 10 minutes of June 2010.
of 0.146 ppmv (Fig. 8). Although neural networks usually are very
effective in dealing with multivariate analysis problems, in this
specific case of TRS emissions for the month of June, the neural
network models were not suitable. As showed in Figure 5, the
best correlation for the best model among all the possible network
architectures was only 0.47. The useful information extracted from
this analysis is again the correlation between TRS emissions and
variables affecting boiler furnace temperature.
The third time period regards the last 53 hours and 10 minutes of the
month of June 2010 that provided a total of 550 data sets. After the
filtering step there remained 514 datasets, corresponding to 93.5% of
data. After the selection of variables that influence the emissions of
CONCLUSIONS
Traditionally TRS emissions are thought to come from low
furnace temperature or poor mixing. This study concluded
that in yearly operation, the parameters related to high furnace
temperature seemed to be the determining ones for TRS emission
in recovery boilers for long term evaluation. However over short
problematic time intervals the transient operating condition
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Fig. 10. Prediction of TRS emission by best neural network model
for the dataset of the last 53 hours and 10 minutes of June 2010.
TRS for this period of time, the R2 coefficients were obtained based
on the analysis of Pearson correlation (Fig. 9). For this period of time
the variables with greatest influence on TRS emissions were also
associated with temperatures and flows of methanol, temperatures
and flows of primary and secondary air, flow of non-condensable
gases, being the first three variables with correlation values over
60%.
The regression variables pre-selected for the development of the
neural model were the ones with correlation above 60%. In total 3
regression variables were obtained, which correspond to 4% of the
total input system variables. Although the main candidate regression
variable that had the most influence on the TRS emissions previously
was the temperature, this was not the case for this dataset. The
predefined variables selected for the development of neural model
for the end of June 2010, when the largest emissions occurred, were
different. These variables were the pressure and flow of methanol in
the burner, and the the flow of non-condensable gases. These three
regression variables can be observed in Table 2.
The best neural network model obtained for the end of the month of
June 2010 was the back propagation with one hidden layer, with four
neurons that showed a correlation of 0.85 and a mean absolute error
of 0.129 ppmv (Fig. 10).
Overall this study shows that in black liquor combustion process, the
furnace temperature is the main variable that influences the TRS
emissions when operation is analysed over a long period of time as
was the case for the data covering the entire year of 2010. Similar
but lower magnitude effect through furnace temperature is from air
preheating. This result is in agreement with the literature. However,
over a short period of time where transient disturbances happen,
other variables like DNCG temperature and flows of alternative fuels
influenced TRS emissions the most. Variables like oxygen content
and furnace pressure vary only during transient operation conditions
such as in the periods of June 2010 analysed in this work. It seems
that during transient operation the TRS emissions are higher than
during steady periods for the mill evaluated.
can lead to sharp increases in TRS emission for a variety of
reasons. Finally, regarding the TRS levels in the dissolving
tank vent scrubber gases, a careful material balance around the
tank identified the source of the problem in the Lincacel plant.
This procedure helps to identify significant sources of sulfur-
containing streams that could be impacting the equipment.
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Original manuscript received 24 July 2013,
revision accepted 21 November 2013