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International Journal of Trend in Scientific Research and Development (IJTSRD)
Volume 3 Issue 5, August 2019 Available Online: www.ijtsrd.com e-ISSN: 2456 – 6470
@ IJTSRD | Unique Paper ID – IJTSRD27841 | Volume – 3 | Issue – 5 | July - August 2019 Page 1805
Statistical Optimization of
Synthetic Soda Ash for Water Softening
Su Mon Tun1, May Myat Khine2, Khin Thidar Cho3
1Lecturer, 2Professor and Head, 3Professor
1Department of Chemical Engineering, Technological University, Mandalay, Myanmar
2,3Department of Chemical Engineering, West Yangon Technological University, Yangon, Myanmar
How to cite this paper: Su Mon Tun | May
Myat Khine | Khin Thidar Cho "Statistical
Optimization of Synthetic Soda Ash for
Water Softening" Published in
International
Journal of Trend in
Scientific Research
and Development
(ijtsrd), ISSN: 2456-
6470, Volume-3 |
Issue-5, August
2019,pp.1805-1812,
https://doi.org/10.31142/ijtsrd27841
Copyright © 2019 by author(s) and
International Journal ofTrend inScientific
Research and Development Journal. This
is an Open Access article distributed
under the terms of
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Commons Attribution
License (CC BY 4.0)
(http://creativecommons.org/licenses/by
/4.0)
ABSTRACT
Synthesized soda ash was prepared by Solvay process with different molar
ratio for application of water softening process. In urban utilization, water
supply is very important for safe condition. In this research, Box-Behnken
experimental design was employed for optimization of soda ash. The
maximum yield percent of 19.882 % of soda ash was obtained by the reaction
salt to ammonium hydroxide to carbon dioxide (1:3:6.8) during the reaction
time 90 min. The synthesized soda ash was analyzed by X-ray diffraction
(XRD), Scanning Electron Microscope (SEM), Energy Dispersive X-ray
Fluorescence (EDXRF) and Fourier Transform Infrared Spectroscopy (FTIR).
Soda ash obtained from optimum condition was applied in water softening of
tap water. According to the experimental results of water softening process,
the maximum removal of hardness of water was observed at 3mlof10% lime
solution with 20 ml of 5 % of soda ash solution for 1000 ml of water. After
treated the lime-soda process, the total hardness of water was reduced to
initial condition of 255 ppm to 24 ppm.
KEYWORDS: Soda Ash, Optimization, Solvay, Water Softening, Total Hardness
I. INTRODUCTION
Soda ash also recognized as sodium carbonate is a white crystalline solidthat
is produced large amount in the world [1].Commercial soda ash is highly
purified and is sold in various grades that differ primarily in bulk density [2].
Sodium carbonate is produced synthetically and from
natural resources. In 2016, 74 % of sodium carbonate was
produced by synthetic method and 26% is from natural
process [2].
The most common way to produce soda ash is Solvay
process which can beproducedbysalt,ammonia,andcarbon
dioxide gas. Reaction time and molar concentration are
important parameters in soda ash manufacturing.
Soda ash is also used in many application such as a pH
regulator , important raw materials in glass manufacturing,
chemicals, soaps and detergents, paper, ceramic materials,
medicines, textiles, steel manufacture, petroleum refining ,
water treatment and other important industrialproducts[1].
Nowadays, statistics plays an important role in research
works and industrial applications. In this research work,
Response Surface Methodology was used inconsideration of
experimental design. The response surface methodology
RSM is a collection of mathematical and statistical
techniques for empirical model buildings, design of
experiments, and evaluating the effects of parameters [3]. In
this research, soda ash was prepared by Box-Behnken
experimental design to obtain optimum condition. The
obtained soda ash was employed in water softeningprocess.
The objectives of water softening is to reduce the adverse
effect of hard water. Hardness of water is caused by calcium
and magnesium ions in water resultings from coming in
contact with geological formations. The hardness interfere
with the laundering ofcausingexcesssoapconsumption,and
may produce scales in small heaters and pipes . To a
considerable extent these advantages have been overcome
by the use of synthetic detergent and lining ofpipes insmall-
hot-water heaters. Industries generallypreheatboiler water
to prevent scaling [4] .
For domestic uses , treated water must be aestheticlly
acceptable free from appearent turbidity , color,
objectionabletaste.Qualityrequirements forindustrials uses
frequently more stringent than domestic supplies [4].
II. MATERIALS AND METHODS
A. Raw Materials
The most important raw materials for preparation of soda
ash are salt, ammonia, and carbon dioxide.
1. Salt: Salt is one of the most important raw materials in
production of synthetic soda ash. It is inexpensive and
easy to collect from local market. In its edible form of
salt, it is commonly used in many industrial processes.
2. Ammonia Solution: Ammonia solution, also known as
ammonia water, is a solution of ammonia inwater.It can
be denoted by the symbols NH3 (aq). It is sometimes
throughout of solution of ammonium hydroxide [5]. In
IJTSRD27841
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this research, 25% of ammonia solutionwas usedas raw
material in soda ash preparation. It can be purchased
from local market.
3. Carbon Dioxide: Carbon dioxide is a colorless gas with
a density about 60% higher than that of dry air. Carbon
dioxide consists of carbon atom covalently doubled
bonded to one oxygen atoms [6]. In this research, it was
used as a raw material in preparation of soda ash.
B. Preparation of Raw Salt
Salt analysis was carried out to determine the specification
of salt before purification. The raw salt composition was
shown in Table. I and analyzed byEDTA titrationmethod [7],
Complex metric titration method [8] and AOAC method [9].
TABLE I.COMPOSITION OF RAW SALT SOLUTION
Specification ppm Methods
Total Hardness 448 EDTA Titration
Total Alkalinity 90 Complexometric Titration
Calcium 4 AOAC
Magnesium 23.04 AOAC
According to the analytical results, salt purification process
was carried out by sedimentation process. The (300) gm of
raw salt was mixed with (1000) ml of water. Andthen,it was
stirred until the salt was completely dissolved. After that, it
was settled to separate the clear solution and sediment.
When the insoluble particles were settled, the clear solution
was passed through the filter to remove the impurities.
Finally, the filtrate was evaporated to 100 ံC, to obtain the
clean salt.
C. Preparation of Synthetic Soda Ash bySolvayprocess
The sodium chloride (25) gm was weighed and mixed with
the 25 %( w/w) of ammonia solution. And then; the mixture
was stirred for a few minutes until all sodium chloride was
completely dissolved. After that, when the carbon dioxide
gas was passed through the solution and the reaction time
was noted. The carbonation reaction was shown in equation
1[10].
NaCl + NH4 OH + CO2 NaHCO3 + NH4Cl (1)
The reaction was proceeded until the significant amount of
precipitates were started to form round about 1 hr. After 15
minutes, the precipitate of sodium bicarbonate was formed.
And then, 15 minutes period was over, the reactor was put
into the ice bath and cooled for 1 hr.
The cooled precipitated sodium bicarbonate was decanted
into the conical flask by passing the clean funnel with
whatman filter paper. And then precipitates were washed
with cooled distilled water to remove unreacted salt and
ammonium chloride. And then, it was calcined in muffle
furnace at a temperature about 200 ံC, carbon dioxide and
water vapor was driven off. The calcinations reaction was
shown in equation 2 [10].
2NaHCO3 Na2CO3 + H2O + CO2 (2)
The calcined soda ash was groundwithmotorandpestleand
finally soda ash was obtained.
According to this experimental procedure, the preliminary
experiments were conducted at molar ratio of 1:1:1, 1:3:3
and 1:6:6 of salt to ammonium hydroxide to carbon dioxide
gas. The experimental procedure for preparationofsoda ash
was shown in Figure .1.
Figure.1. Preparation of Synthesized Soda Ash
III. RESULTS AND DICUSSIONS
According to the preliminary experiments, the yield percent
of soda ash was described in Table (II). Moreover, statistical
designs were considered to provide the optimizationofsoda
ash.
TABLE II. YIELD % OF SODA ASH FROM PRELIMINARY
EXPERIMENTS
Experiment
No
Molar Ratio
of NaCl:
NH4OH : CO2
Reaction
time(min)
Yield
%
1 1:1:1 90 9.72%
2 1:3:3 90 19.63%
3 1:6:6 90 16.9%
According to the yield percent of soda ash from preliminary
experiments, independent variables and levels were
considered and selected for design of experiment.Thelevels
for each variable were shown in Table III. The experimental
results were analyzed by ANOVA and the general equation
which satisfied the statistical optimizationwas second order
polynomial equation which was described as follow.
Y = β + ∑ β x + ∑ β x + ∑ ∑ β x x + ε (3)
[3]
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Where, Y is the predicated response of the yield % of soda
ash, xi, xj are the independent variables, β ,β ,β ,β are the
regression coefficient of intercept, linear, quadratic and
interaction effects respectively and εistherandom error [3].
The experimental runs generated with yield percent of soda
ash were shown in table (IV). The analysis ofvarianceforthe
experimental results was shown in table (V).
TABLE III INDEPENDENT VARIABLES AND LEVELS FOR BOX-BEHNKEN DESIGN
Variables Symbols
Level
(-1) (0) (1)
Ammonium Hydroxide (mol) X1 3 4.5 6
Carbon Dioxide (mol) X2 3 7.5 12
Reaction Time (min) X3 90 135 180
TABLE IV BOX-BEHNKEN DESIGN MATRIX, EXPERIMENTAL YIELD % AND PREDICTED YIELD % OF SODA ASH
No Run No X1 X2 X3 Experimental Yield % Predicted Yield %
1 1 -1 0 1 9.60 9.42
2 2 0 -1 1 6.60 6.47
3 3 0 1 -1 1.70 1.83
4 4 -1 0 -1 22.12 19.88
5 5 1 0 1 15.68 17.92
6 6 -1 1 0 0.36 2.46
7 7 1 1 0 0.20 -0.10
8 8 -1 -1 0 6.62 6.50
9 9 0 0 0 4.34 4.34
10 10 1 -1 0 0.12 -1.98
11 11 1 0 -1 0.16 0.33
12 12 0 0 0 4.04 4.34
13 13 0 0 0 4.64 4.34
14 14 0 1 1 6.40 4.46
15 15 0 -1 -1 0.04 1.97
TABLE V. ANALYSIS OF VARIANCE FOR YIELD % OF SODA ASH
Source DF SS Adj MS F value P value R2 R2
adj
Regression 9 532.768 59.196 11.03 0.008 95.20 % 86.57%
linear 3 88.892 29.631 5.52 0.048
Square 3 237.690 79.230 14.76 0.006
Interaction 3 206.187 68.729 12.80 0.009
Error 5 26.841 5.368 - -
Lack of fit 3 26.661 8.887 98.74 0.01
Pure Error 2 0.180 0.090 -
Yield % = 129.3 - 28.68 X1 + 3.21 X2 - 62.7 X3 + 1.241 X1
2 - 0.2673 X2
2 + 8.46 X3
2 + 0.219 X1X2+ 6.23 X1X3 - 0.138 X2X3 (4)
F-value and P-value were used to check the significance of
the model. According to the ANOVA table , the P-value of the
model was less than 0.05, which described that it was a
significant model. Based on 95 % confidence level , the
model was confirmed to be significant as the computed F
value , (11.03) was much higher than that the theoretical F
value ,F0.05:(9,5)(4.77). The high value of R2 and R2
adj
representing the high degree of correlation between the
experimental yield % and predicted yield %. The coefficient
of determinations (R2) was 95.20 % which indicated thatthe
model was significantly effected and represented the real
relationship among the parameters.So ,it can be said a fitted
model [11] .
The optimum value of 19.882 % was obtained at molar ratio
of salt to ammonium hydroxide to carbon dioxide 1:3: 6.8
and reaction time 1.50 hr. When this optimization was
validated with the experiment, it gave percent conversionof
yield percent of 19 %.It can be found that error percent of
4.4 which was acceptable within the range of 95 %
confidence level.
D. Characterizations of Soda Ash
The products were analyzed by X-ray diffraction (XRD),
Scanning Electron Microscopy (SEM), Energy Dispersive X-
rays Fluorescence (EDXRF),andFourierTransform-Infrared
Spectroscopy (FTIR).
1. X-ray diffraction (XRD)
The XRD patterns of soda ash from experiment 1,
experiment 2, expriment 3 and optimum condition of soda
ash from Box- Behnken experimental design was shown in
Figure. 2 .They were compared to standard soda ash.
According to the XRD patterns, experiment 1 , experiment 2
and experiment 3 have thirteen characteristic peaks.
However the soda ash which prepared by optimum
condition of Box-Behnken experimental design was more
clear and favorable.It has thirteen characteristics peaks and
observed at angle 2 𝜃(27.188) , (29.953), (34.021),(33.082),
(34.354), (35.055), (37.736), (39.705), (41.215), (41.460),
(53.423), (56.874), (62.419) were corresponding to (201),
(002), (020), (-202), (-112), (310), (112), (202), (400), (-
International Journal of Trend in Scientific Research and Development (IJTSRD)
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221), (222), (402) and (-601).The highest intensities peaks
of soda ash from optimum condition was occurred at 2
37.736) and 2 𝜃 (29.953). According to the XRD
product was said to soda ash.
Figure.2. XRD patterns of Synthetic Soda Ash
2. Scanning Electron Microscopy (SEM)
In this study ,the morphology of synthetic soda ash were
determined by Sacnning Electron Microscopy (SEM).
SEM images of soda ash from expermient 1, 2 and 3 were
shown in Fig. 3,4 and 5. According to the
experiment 1 and experiment 2 were rod shape and they
were aggregated to each other. The SEM image from
experiment 3 was cylindrical shape.The morphology of
image of soda ash from optimum condition was shown in
Fig.6. It was more aggregate and fine than experiment 1,
experiment 2 and 3. According to the SEM images , the
shapes of soda ash samples were generally in
they were formed as crystalline structure. Some of them
were aggregated and some were scattered.
Figure.3. SEM image of Soda Ash from Experiment 1
Figure.4. SEM image of Soda Ash from Experiment 2
Optimal Condition
Experiment
Experiment
Experiment
Standard soda ash
Optimum Condition
Experiment
Experiment
Experiment
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27841 | Volume – 3 | Issue – 5 | July - August 2019
hest intensities peaks
from optimum condition was occurred at 2 𝜃(
(29.953). According to the XRD patterns, the
2. XRD patterns of Synthetic Soda Ash
Scanning Electron Microscopy (SEM)
In this study ,the morphology of synthetic soda ash were
by Sacnning Electron Microscopy (SEM). The
SEM images of soda ash from expermient 1, 2 and 3 were
shown in Fig. 3,4 and 5. According to the SEM images,
experiment 1 and experiment 2 were rod shape and they
were aggregated to each other. The SEM image from
experiment 3 was cylindrical shape.The morphology of SEM
image of soda ash from optimum condition was shown in
more aggregate and fine than experiment 1,
experiment 2 and 3. According to the SEM images , the
nerally in rod shape and
structure. Some of them
were aggregated and some were scattered.
Figure.3. SEM image of Soda Ash from Experiment 1
Figure.4. SEM image of Soda Ash from Experiment 2
Figure. 5. SEM image of Soda Ash from Experiment 3
Figure.6 SEM image of Soda Ash from Optimum
Condition
3. Energy Dipersive X-ray Fluorescence (EDXRF)
Quantitative results of soda ash were analyzed by using
Energy DipersiveX-rays Fluorescence(EDXRF).Accordingto
the EDXRF results, carbon percent from experiment (1) ,
experiment (2) and experiment (3) were 92.64% , 93.73%
and 92.53 % respectively . Sodium percent from experiment
(1), experiment (2) and experiment (3) were 7.07 % , 6.08%
and 7.27% respectively. According to t
results, the optimnum condition ofsoda ashwas
Fourier Transform Infread Spetroscopy (FTIR).
4. Fourier Transform Infrared Spectroscopy (FTIR)
The optimum conditionofsoda ashpepared by Box
experimental design was analyzed by Fourier Transform
Infrared Spectroscopy .The spectra was recorded in the
range (500- 4000 cm -1) . According to the infrared spectrum
of soda ash , the stretching bonds of (O
approximately 3500 cm-1 and 3000 cm
have been attributed to hydroxyl group.The stretchingbond
of (C-O) was occurred at 1454.38 cm
of (C-CL) was occurred at 858.38 cm
impurities in the sample.The infrared spectrum of soda ash
from optimum condition is nearly the same as
soda ash [11].
Wavelength (cm
Figure.7. Infrared Spectrum of Standard Soda Ash[1
ptimal Condition
Experiment - 3
Experiment - 2
Experiment -1
soda ash
Optimum Condition
Experiment -3
Experiment -2
xperiment -1
T
%
85
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August 2019 Page 1808
Soda Ash from Experiment 3
SEM image of Soda Ash from Optimum
Condition
ray Fluorescence (EDXRF)
Quantitative results of soda ash were analyzed by using
rays Fluorescence(EDXRF).Accordingto
results, carbon percent from experiment (1) ,
experiment (2) and experiment (3) were 92.64% , 93.73%
and 92.53 % respectively . Sodium percent from experiment
(1), experiment (2) and experiment (3) were 7.07 % , 6.08%
and 7.27% respectively. According to the experimental
results, the optimnum condition ofsoda ashwas analyzedby
Fourier Transform Infread Spetroscopy (FTIR).
Fourier Transform Infrared Spectroscopy (FTIR)
soda ashpepared by Box-Behnken
experimental design was analyzed by Fourier Transform
Infrared Spectroscopy .The spectra was recorded in the
) . According to the infrared spectrum
of soda ash , the stretching bonds of (O-H) were observed at
and 3000 cm-1respectively and
have been attributed to hydroxyl group.The stretchingbond
occurred at 1454.38 cm -1 .The stretching bond
occurred at 858.38 cm-1 that is due to the
ample.The infrared spectrum of soda ash
from optimum condition is nearly the same as the standard
Wavelength (cm-1)
Figure.7. Infrared Spectrum of Standard Soda Ash[1
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Figure.8. Infrared Spectrum of Soda Ash from
Optimum Condition
E. Application of Soda Ash
According to the analytical results of the synthetic soda ash ,
it was confirmed as soda ash. It was applied in water
softening process for removal of total harhness of water.
Water sample was taken from the laboratory of Chemical
Engineering Department from West YangonTechnological
University Campus, Hlaing Tharyar Township, Yangon
Region.Water analysis was carried out by APHA standard
methods. The charaterization of raw water was shown in
Table(VI).
TABLE(VI).Characterization of Raw Water
No Specifications Value
1 Total Hardness(ppm) 255
2 Total Alkalinity(ppm) 85
3 Calcium(ppm) 47
4 Magnesium(ppm) 4.37
5 Sulfate(ppm) 43.1
6 Chloride(ppm) 400
7 Iron(ppm) 28
8 pH 7.9
F. Water Softening
1. Precipitatives Softening
Precipitative softening uses lime (Ca(OH)2) and soda ash
(Na2CO3) to remove calcium and magnesium ions from
solution. Lime added to water reacts first with free carbon
dioxide forming a calcium carbonate precipitate .The lime
reacts with free carbon dioxide forming a calcium
bicarbonate present . In both of these equation one
equivalent of lime reacts with free carbon dioxide forming a
calcium carbonate precipitate. The lime reacts with any
calcium bicarbonate present. In both of these equations,one
equivalent of lime combines with one equivalent of either
CO2 or Ca(HCO3)2 .
CO2 + Ca(OH)2 CaCO3 + H2O (4) [4]
Ca(HCO3)2 + Ca(OH)2 2CaCO3 + 2H2O (5) [4]
Since magnesium precipitates as Mg(OH)2
Mg (HCO3)2 + Ca(OH)2 MgCO3 + CaCO3 + 2H2O (6) [4]
MgCO3 + Ca (OH)2 Mg (OH)2 + CaCO3 (7) [4]
MgSO4 + Ca(OH)2 CaSO4 + Mg(OH) (8) [4]
Lime- soda softening
Removal of Carbonate hardness with lime
Ca2+ + 2HCO3
- + Ca (OH)2 2CaCO3 + 2H2O (9) [13]
Mg2+ + 2HCO3 + 2Ca(OH)2 2CaCO3 + Mg(OH)2 + H2O(10)
[13]
Removal of non-carbonate hardness with soda ash and lime
Ca2+ + 2Cl- +Na2CO3 CaCO3 + 2Na+ +2Cl- (11) [13]
Ca2+ + SO4
2- + Na2CO3 CaCO3 + 2Na+ + SO4
2- (12) [13]
Mg2+ + 2Cl- + Ca(OH)2 Mg(OH)2 + Ca2++ 2Cl- (13) [13]
Mg2++ SO4
2-+ Ca(OH) Mg(OH)2 +Ca2++ SO4
2- (14)[13]
Recarbonation for pH Control
CO3
2- + CO2+ H2O 2HCO2
3
- (15) [13]
In this research , water soft ening process was carriedout by
various dosage of lime and soda ash.Experiment (I)was
carried out by single-stage lime-softening process.
Experiment (II) was carried out by synthesized soda ash.
Experiment (III) was carried out by watersoftening byusing
both lime and synthesized soda ash. Experiment (IV) was
carried out by water softening by using both lime and
commercial soda ash.
1. Procedure of Water Softening with Lime
In experiment I , raw water (100) ml was taken to treat with
10 % lime solutuion (Ca(OH)2). And then , it was stirred by
magnetic stirrer with 500 rpm. After that it was settled for
10 min. The lime treated water was passed throughthefilter
paper and pH was measured before and after filtration.
According to this experiment, when the lime dosage was
increased, the pH of water was increased from initial
condition to pH 9. On the other hand, total hardness was
decreased from initial condition of 255 ppmto229,200,242
ppm respectively. According to the experimentalresults,the
optimum condition was observed at0.3mloflimefor100ml
of sample water. The effect of various dosage of lime vs total
hardness and pH was shown in Figure 8.
Figure.8. Effect ot of Total Hardness and pH with
various dosage of Lime Solution
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According to this graph, whenlimedosagewas increased, pH
was steadily increased. However, lime dosage was exceeded
over the required level, hardness of water was returned to
increase . According to this graph , only lime solutioncannot
reduced the total hardness significantly.
2. Procedure of Water Softening Process With
Synthesized Soda Ash
In experiment (II) , raw water (100) ml was taken to treat
with 5 % synthesized soda ash solution . And then it was
stirred by magnetic stirrer with 500 rpm. After that , it was
settled for 10 min and passed through a filter paper. The
soda ash treated water was analyzed by EDTA titration
method to know the removal efficiency of total hardness.
According to the experimental results , hardness of water
was effected by various dosage of soda ash.When thedosage
was increased , the pH of water was significantly increased.
So , the hardness and pH of water were inversely
proportional according to the dosage of soda ash. However,
the dosage of synthesized soda ash was exceeded over the
required level , hardness level of water was increased
significantly. The effect of synthesized soda ash vs total
hardness and pH was shown in Figure.9.
Figure.9. Effect of Total Hardness and pH with Various
Dosage of Synthesized Soda Ash Solution
According this graph, pH level was sharply raised when the
dosage was increased. The hardness of water was
significantly decreased from initial condition of 255 ppm to
171 ppm. However, hardness level was returned to increase
when the dosage was increased.
3. Procedure of Water Softening Using Both Lime and
Synthesized Soda Ash
In experiment (III ) , water sample was treatedby using both
lime and synthesized soda ash. According to the lime
process, 0.3 ml of lime was taken as optimum condition
because which removed the hardness than other dosage.
According to the lime dosage, the pH level of water was
raised; the bicarbonates ions were converted to carbonate
concentration. Due to the increase in carbonate
concentration, precipitates of calcium carbonate were
formed. The remaining calcium cannot be removed by
simple adjustment of pH. So, soda ash solution was addedby
varying the dosage to precipitates the remaining calcium. In
lime-soda treatment, the pH level was raised by addition of
lime while sodium carbonate was added to reduce residual
carbonate hardness. The treated water was passed through
the filter paper, and then it was analyzed by EDTA titration
method.
According to the experiment, lime and various dosage of
synthesized soda ash was effectively reduced the water
hardness. Maximum removal percent of hardness of water
was observed at 0.3 ml of lime and 2 ml of synthesized soda
ash. The effect of both lime and soda ash dosage vs pH and
total hardness was shown in Fig. 10.
Figur.10. Effectof Lime-Soda Dosage by Synthesized
Soda Ash
According to this graph , hardness of waterwas dramatically
decreased but pH of water was increased. When the dosage
of was increased over the required level, the hardnesslevel
of water was slightly increased.
4. Procedure of Water Softening Using Both Lime and
Commercial Soda Ash
In experiment IV, lime-soda softening process was carried
out using the commercial grade soda ash to reduce the
hardness of water. The procedure was the same as using the
lime and various synthesized soda ash.
According to the results, water softening by using both lime
and commercial soda ash dosage effectively reduced the
water hardness. The maximumremoval ofhardnessofwater
was observed at 0.3 ml of lime and 2ml of commercial soda
ash. The effect of lime and soda ash dosage on pH and total
hardness was shown in Figure 11.
Figur11.Effect of lime and various dosage of
commercial soda ash
According to this graph, hardness of water was dramatically
decreased but pH of water was increased. When the dosage
was increased over the required level, the hardness level of
water was slightly increased.
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5. Jar Testing
Firstly, one liter of sample water was taken and added to
each of the beakers of gang-mixersystem.Themixers in each
beaker were allowed to set a mixing rate of 150 rpm. Next,
5% of commercial grade sodium carbonate solution was
added into the first beaker. And then, 5% of synthesized
soda ash solution was added into the second beaker and
allowed to mix with 150 rpm. According to the lime-soda
softening process, the optimum condition of 3 ml of lime
solution was added into the third and fourth beakers. After
10 minutes, the beakers were allowed to settle. Following
the settling period, the samples were collected from each
beaker and filtered. The pH levels were measured for
adjusting the optimum range.
After that, 5% synthesized soda ash solution was added into
lime treated water by varying dosage. The mixers in each
beaker were allowed to set up the 150 rpm. After 10
minutes, the beakers were allowed to settle for 10 minutes.
After settling, the samples were filtered. The pH was
measured before and after filtration. And then it was passed
through by carbon dioxide gas to obtain the acceptable pH
range of (6.5- 8.5). Finally, the treated waters were
measured pH and total hardness.
According to the jar testing results, lime-soda softening
process was more effectively reduced the hardness of water
than only synthesized soda ash dosage. Water softening by
using both synthesized soda ash dosage and lime is more
effective. According to the lime-soda softening process, the
optimum condition for one liter water was observed at 3 ml
of lime and 20 ml of synthesized soda ash. And then, the
treated water from the optimum condition was passed
through by carbon dioxide to obtain acceptable pH range of
6.5 ~ 8.5. Finally, it was measured to total hardness, total
alkalinity, calcium, magnesium, sulfate, chloride and iron.
The result of treated water by jar test was shown in Table
VII. The Specifications of treated water was shown in Table
VIII.
Table VII. JAR Testing Results
Run No
Volume of
Sample
Water (ml)
10% lime
Solution
5%Soda Ash Solution (ml) Settling
Tim(min)
pH
Total
Hardness
Hardness
Removal
%Synthesized Commercial
1 1000 - 20 - 10 9 185 27.45
2 1000 - - 20 10 9 175 31.72
3 1000 3 20 - 10 9.5 24 90.59
4 1000 3 10 -- 10 9 26 89.80
TABLE VIII SPECIFICATION OF TREATED WATER
No Specifications Raw Water Value Treated Water Value
1 Total Hardness(ppm) 255 24
2 Total Alkalinity (ppm) 85 240
3 Calcium(ppm) 47 9.02
4 Magnesium(ppm) 4.37 0.2
5 Sulfate(ppm) 43.1 45.2
6 Chloride(ppm) 400 370
7 Iron(ppm) 28 <
8 pH 7.9 6.5
According to the experimental results, the concentration of
raw water and the treated water were different. Lime-soda
softening process was reduced the hardness from initial
concentration of 255 pm to 24 ppm. However, the total
alkalinity was increased from initial condition of 85 ppm to
240 ppm according to the lime dosage. Calcium, magnesium
and iron were dramatically reduced from initial
concentrations because of lime and soda ash dosage. Sulfate
was slightly increased from initial concentration of 43.1 to
45.2 ppm. Chloride was slightly reduced from 400 ppm to
370 according to lime-soda dosage. Before carbonation, pH
of treated water is 9.5; it was reduced to pH 6.5 by passing
carbon dioxide gas. It was within the acceptable level. The
initial pH of raw water is 7.9.The final pH of treated water
was 6.5.
IV. CONCLUSIONS
In this study, the soda ash is prepared synthetically by
Solvay process by the use of Box-Behnken experimental
design. The maximum yield percent of 19.882% was
obtained with the reaction salt to ammonium hydroxide to
carbon dioxide ratio of 1:3:6.8 during reaction time 90
minutes. According to the XRD patterns, SEM images and
FTIR result, the optimum condition which prepared by Box-
Behnken experimental design is said tosoda ashand applied
in water softening process.
Water softening was carried out by lime softening,softening
by synthesized soda ash, softening by commercial soda ash
and lime-soda softening process. According to the
experimental results, lime softening process cannot
adequately reduce the hardness level. Softening by
synthesized and commercial soda ash can reduce the
hardness level of water.
However, the lime-soda process can effectively reduce the
hardness level of water. The initial characteristics of raw
water is total hardness of 255 ppm, total alkalinity of 85
ppm, calcium of 47 ppm , magnesium of 4.37 ppm , sulfate of
43.1 ppm , chloride of 400 ppm , iron of 28 ppm. The initial
pH is 7.9. After lime-soda treatment, thetotalhardness of 24,
total alkalinity of 240, Calcium of 9.02, Magnesium of 0.2,
Sulfate of 45.2%, Chloride of 270, Iron of < 0.1 and pH of 6.5
are obtained.
International Journal of Trend in Scientific Research and Development (IJTSRD) @ www.ijtsrd.com eISSN: 2456-6470
@ IJTSRD | Unique Paper ID – IJTSRD27841 | Volume – 3 | Issue – 5 | July - August 2019 Page 1812
ACKNOWLEDGEMENT
The author would like to express her thankstoallprofessors
and all lecturers of Chemical Ennginering Department,West
Yangon Technological University for giving the opportunity
to carry out this reseasrch. And also the author is deeply
gratitude to professors for their kind advice and systematic
guidance . Finally, the author is particularly indebted to
Chairman of Green Myanmar Environmental Services for
financial support and lab facility for preparing this research.
RFERENCES
[1] T. Madima , “ Manufcturing of Synthetic Sol da Ash,”
M.S.c thesis,University of the Cape, South Africa,
Feb.2009
[2] K..E McCaleb , TheBiography of a Chemical Economic
Handbook Report ,Chemical Information Services,
Stanford Research Institute, Melno- Park ,Calif.94025 ,
Nov. 1971
[3] R. H. MyersandD. C. Montgomery, “Response Surface
Methodoloy,” 3rd Edition,2008
[4] Aung Myint Soe , “ ChT-2024, Introduction to Chemical
Technology” Lecture Note, 2003, Department ot
Chemical Engineering , Yangon Technological
University
[5] Housecroft, C.E and Sharpe, A.G. 2004. Inorganic
Chemistry. 2nd edition. Prentice Hall. P187
[6] Air Products and Chemicals (APC), Inc,2009 . “Carbon
Dioxide”Product Stewardship Summary
[7] M.C.RAND, A.E.GREENBERG, M. J. TARAS , “Standards
Methods For the Examination of Water and Waste
Water,” 14 th edition
[8] Dr. G. W.Latimer, Jr, “Officials Methods of Analysis
ofAOAC International , ” 20th edition, 2016
[9] ESEPA- European Soda Ash Procedure Association ,
“Process BREF For Soda Ash” ,March 2004.
[10] R.A.Meyers (Ed.), Encylopedia of Analytical Chemistry,
pp.10815-10837, 2000
[11] Anonymous ,”Sodium Carbonate, Database of ART-
FT_IR spectra of various materials<
lisa_Chem_ut.ee>IR_spectra>paint> paint>fillers
[12] Dipa Dey,Amanda Herzog, Vidya Srinivaszn,“Chemical
Precpitation: “Water Softening” , ENE806, May 2 ,2007

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Statistical Optimization of Synthetic Soda Ash

  • 1. International Journal of Trend in Scientific Research and Development (IJTSRD) Volume 3 Issue 5, August 2019 Available Online: www.ijtsrd.com e-ISSN: 2456 – 6470 @ IJTSRD | Unique Paper ID – IJTSRD27841 | Volume – 3 | Issue – 5 | July - August 2019 Page 1805 Statistical Optimization of Synthetic Soda Ash for Water Softening Su Mon Tun1, May Myat Khine2, Khin Thidar Cho3 1Lecturer, 2Professor and Head, 3Professor 1Department of Chemical Engineering, Technological University, Mandalay, Myanmar 2,3Department of Chemical Engineering, West Yangon Technological University, Yangon, Myanmar How to cite this paper: Su Mon Tun | May Myat Khine | Khin Thidar Cho "Statistical Optimization of Synthetic Soda Ash for Water Softening" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456- 6470, Volume-3 | Issue-5, August 2019,pp.1805-1812, https://doi.org/10.31142/ijtsrd27841 Copyright © 2019 by author(s) and International Journal ofTrend inScientific Research and Development Journal. This is an Open Access article distributed under the terms of the Creative Commons Attribution License (CC BY 4.0) (http://creativecommons.org/licenses/by /4.0) ABSTRACT Synthesized soda ash was prepared by Solvay process with different molar ratio for application of water softening process. In urban utilization, water supply is very important for safe condition. In this research, Box-Behnken experimental design was employed for optimization of soda ash. The maximum yield percent of 19.882 % of soda ash was obtained by the reaction salt to ammonium hydroxide to carbon dioxide (1:3:6.8) during the reaction time 90 min. The synthesized soda ash was analyzed by X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Energy Dispersive X-ray Fluorescence (EDXRF) and Fourier Transform Infrared Spectroscopy (FTIR). Soda ash obtained from optimum condition was applied in water softening of tap water. According to the experimental results of water softening process, the maximum removal of hardness of water was observed at 3mlof10% lime solution with 20 ml of 5 % of soda ash solution for 1000 ml of water. After treated the lime-soda process, the total hardness of water was reduced to initial condition of 255 ppm to 24 ppm. KEYWORDS: Soda Ash, Optimization, Solvay, Water Softening, Total Hardness I. INTRODUCTION Soda ash also recognized as sodium carbonate is a white crystalline solidthat is produced large amount in the world [1].Commercial soda ash is highly purified and is sold in various grades that differ primarily in bulk density [2]. Sodium carbonate is produced synthetically and from natural resources. In 2016, 74 % of sodium carbonate was produced by synthetic method and 26% is from natural process [2]. The most common way to produce soda ash is Solvay process which can beproducedbysalt,ammonia,andcarbon dioxide gas. Reaction time and molar concentration are important parameters in soda ash manufacturing. Soda ash is also used in many application such as a pH regulator , important raw materials in glass manufacturing, chemicals, soaps and detergents, paper, ceramic materials, medicines, textiles, steel manufacture, petroleum refining , water treatment and other important industrialproducts[1]. Nowadays, statistics plays an important role in research works and industrial applications. In this research work, Response Surface Methodology was used inconsideration of experimental design. The response surface methodology RSM is a collection of mathematical and statistical techniques for empirical model buildings, design of experiments, and evaluating the effects of parameters [3]. In this research, soda ash was prepared by Box-Behnken experimental design to obtain optimum condition. The obtained soda ash was employed in water softeningprocess. The objectives of water softening is to reduce the adverse effect of hard water. Hardness of water is caused by calcium and magnesium ions in water resultings from coming in contact with geological formations. The hardness interfere with the laundering ofcausingexcesssoapconsumption,and may produce scales in small heaters and pipes . To a considerable extent these advantages have been overcome by the use of synthetic detergent and lining ofpipes insmall- hot-water heaters. Industries generallypreheatboiler water to prevent scaling [4] . For domestic uses , treated water must be aestheticlly acceptable free from appearent turbidity , color, objectionabletaste.Qualityrequirements forindustrials uses frequently more stringent than domestic supplies [4]. II. MATERIALS AND METHODS A. Raw Materials The most important raw materials for preparation of soda ash are salt, ammonia, and carbon dioxide. 1. Salt: Salt is one of the most important raw materials in production of synthetic soda ash. It is inexpensive and easy to collect from local market. In its edible form of salt, it is commonly used in many industrial processes. 2. Ammonia Solution: Ammonia solution, also known as ammonia water, is a solution of ammonia inwater.It can be denoted by the symbols NH3 (aq). It is sometimes throughout of solution of ammonium hydroxide [5]. In IJTSRD27841
  • 2. International Journal of Trend in Scientific Research and Development (IJTSRD) @ www.ijtsrd.com eISSN: 2456-6470 @ IJTSRD | Unique Paper ID – IJTSRD27841 | Volume – 3 | Issue – 5 | July - August 2019 Page 1806 this research, 25% of ammonia solutionwas usedas raw material in soda ash preparation. It can be purchased from local market. 3. Carbon Dioxide: Carbon dioxide is a colorless gas with a density about 60% higher than that of dry air. Carbon dioxide consists of carbon atom covalently doubled bonded to one oxygen atoms [6]. In this research, it was used as a raw material in preparation of soda ash. B. Preparation of Raw Salt Salt analysis was carried out to determine the specification of salt before purification. The raw salt composition was shown in Table. I and analyzed byEDTA titrationmethod [7], Complex metric titration method [8] and AOAC method [9]. TABLE I.COMPOSITION OF RAW SALT SOLUTION Specification ppm Methods Total Hardness 448 EDTA Titration Total Alkalinity 90 Complexometric Titration Calcium 4 AOAC Magnesium 23.04 AOAC According to the analytical results, salt purification process was carried out by sedimentation process. The (300) gm of raw salt was mixed with (1000) ml of water. Andthen,it was stirred until the salt was completely dissolved. After that, it was settled to separate the clear solution and sediment. When the insoluble particles were settled, the clear solution was passed through the filter to remove the impurities. Finally, the filtrate was evaporated to 100 ံC, to obtain the clean salt. C. Preparation of Synthetic Soda Ash bySolvayprocess The sodium chloride (25) gm was weighed and mixed with the 25 %( w/w) of ammonia solution. And then; the mixture was stirred for a few minutes until all sodium chloride was completely dissolved. After that, when the carbon dioxide gas was passed through the solution and the reaction time was noted. The carbonation reaction was shown in equation 1[10]. NaCl + NH4 OH + CO2 NaHCO3 + NH4Cl (1) The reaction was proceeded until the significant amount of precipitates were started to form round about 1 hr. After 15 minutes, the precipitate of sodium bicarbonate was formed. And then, 15 minutes period was over, the reactor was put into the ice bath and cooled for 1 hr. The cooled precipitated sodium bicarbonate was decanted into the conical flask by passing the clean funnel with whatman filter paper. And then precipitates were washed with cooled distilled water to remove unreacted salt and ammonium chloride. And then, it was calcined in muffle furnace at a temperature about 200 ံC, carbon dioxide and water vapor was driven off. The calcinations reaction was shown in equation 2 [10]. 2NaHCO3 Na2CO3 + H2O + CO2 (2) The calcined soda ash was groundwithmotorandpestleand finally soda ash was obtained. According to this experimental procedure, the preliminary experiments were conducted at molar ratio of 1:1:1, 1:3:3 and 1:6:6 of salt to ammonium hydroxide to carbon dioxide gas. The experimental procedure for preparationofsoda ash was shown in Figure .1. Figure.1. Preparation of Synthesized Soda Ash III. RESULTS AND DICUSSIONS According to the preliminary experiments, the yield percent of soda ash was described in Table (II). Moreover, statistical designs were considered to provide the optimizationofsoda ash. TABLE II. YIELD % OF SODA ASH FROM PRELIMINARY EXPERIMENTS Experiment No Molar Ratio of NaCl: NH4OH : CO2 Reaction time(min) Yield % 1 1:1:1 90 9.72% 2 1:3:3 90 19.63% 3 1:6:6 90 16.9% According to the yield percent of soda ash from preliminary experiments, independent variables and levels were considered and selected for design of experiment.Thelevels for each variable were shown in Table III. The experimental results were analyzed by ANOVA and the general equation which satisfied the statistical optimizationwas second order polynomial equation which was described as follow. Y = β + ∑ β x + ∑ β x + ∑ ∑ β x x + ε (3) [3]
  • 3. International Journal of Trend in Scientific Research and Development (IJTSRD) @ www.ijtsrd.com eISSN: 2456-6470 @ IJTSRD | Unique Paper ID – IJTSRD27841 | Volume – 3 | Issue – 5 | July - August 2019 Page 1807 Where, Y is the predicated response of the yield % of soda ash, xi, xj are the independent variables, β ,β ,β ,β are the regression coefficient of intercept, linear, quadratic and interaction effects respectively and εistherandom error [3]. The experimental runs generated with yield percent of soda ash were shown in table (IV). The analysis ofvarianceforthe experimental results was shown in table (V). TABLE III INDEPENDENT VARIABLES AND LEVELS FOR BOX-BEHNKEN DESIGN Variables Symbols Level (-1) (0) (1) Ammonium Hydroxide (mol) X1 3 4.5 6 Carbon Dioxide (mol) X2 3 7.5 12 Reaction Time (min) X3 90 135 180 TABLE IV BOX-BEHNKEN DESIGN MATRIX, EXPERIMENTAL YIELD % AND PREDICTED YIELD % OF SODA ASH No Run No X1 X2 X3 Experimental Yield % Predicted Yield % 1 1 -1 0 1 9.60 9.42 2 2 0 -1 1 6.60 6.47 3 3 0 1 -1 1.70 1.83 4 4 -1 0 -1 22.12 19.88 5 5 1 0 1 15.68 17.92 6 6 -1 1 0 0.36 2.46 7 7 1 1 0 0.20 -0.10 8 8 -1 -1 0 6.62 6.50 9 9 0 0 0 4.34 4.34 10 10 1 -1 0 0.12 -1.98 11 11 1 0 -1 0.16 0.33 12 12 0 0 0 4.04 4.34 13 13 0 0 0 4.64 4.34 14 14 0 1 1 6.40 4.46 15 15 0 -1 -1 0.04 1.97 TABLE V. ANALYSIS OF VARIANCE FOR YIELD % OF SODA ASH Source DF SS Adj MS F value P value R2 R2 adj Regression 9 532.768 59.196 11.03 0.008 95.20 % 86.57% linear 3 88.892 29.631 5.52 0.048 Square 3 237.690 79.230 14.76 0.006 Interaction 3 206.187 68.729 12.80 0.009 Error 5 26.841 5.368 - - Lack of fit 3 26.661 8.887 98.74 0.01 Pure Error 2 0.180 0.090 - Yield % = 129.3 - 28.68 X1 + 3.21 X2 - 62.7 X3 + 1.241 X1 2 - 0.2673 X2 2 + 8.46 X3 2 + 0.219 X1X2+ 6.23 X1X3 - 0.138 X2X3 (4) F-value and P-value were used to check the significance of the model. According to the ANOVA table , the P-value of the model was less than 0.05, which described that it was a significant model. Based on 95 % confidence level , the model was confirmed to be significant as the computed F value , (11.03) was much higher than that the theoretical F value ,F0.05:(9,5)(4.77). The high value of R2 and R2 adj representing the high degree of correlation between the experimental yield % and predicted yield %. The coefficient of determinations (R2) was 95.20 % which indicated thatthe model was significantly effected and represented the real relationship among the parameters.So ,it can be said a fitted model [11] . The optimum value of 19.882 % was obtained at molar ratio of salt to ammonium hydroxide to carbon dioxide 1:3: 6.8 and reaction time 1.50 hr. When this optimization was validated with the experiment, it gave percent conversionof yield percent of 19 %.It can be found that error percent of 4.4 which was acceptable within the range of 95 % confidence level. D. Characterizations of Soda Ash The products were analyzed by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X- rays Fluorescence (EDXRF),andFourierTransform-Infrared Spectroscopy (FTIR). 1. X-ray diffraction (XRD) The XRD patterns of soda ash from experiment 1, experiment 2, expriment 3 and optimum condition of soda ash from Box- Behnken experimental design was shown in Figure. 2 .They were compared to standard soda ash. According to the XRD patterns, experiment 1 , experiment 2 and experiment 3 have thirteen characteristic peaks. However the soda ash which prepared by optimum condition of Box-Behnken experimental design was more clear and favorable.It has thirteen characteristics peaks and observed at angle 2 𝜃(27.188) , (29.953), (34.021),(33.082), (34.354), (35.055), (37.736), (39.705), (41.215), (41.460), (53.423), (56.874), (62.419) were corresponding to (201), (002), (020), (-202), (-112), (310), (112), (202), (400), (-
  • 4. International Journal of Trend in Scientific Research and Development (IJTSRD) @ IJTSRD | Unique Paper ID – IJTSRD2 221), (222), (402) and (-601).The highest intensities peaks of soda ash from optimum condition was occurred at 2 37.736) and 2 𝜃 (29.953). According to the XRD product was said to soda ash. Figure.2. XRD patterns of Synthetic Soda Ash 2. Scanning Electron Microscopy (SEM) In this study ,the morphology of synthetic soda ash were determined by Sacnning Electron Microscopy (SEM). SEM images of soda ash from expermient 1, 2 and 3 were shown in Fig. 3,4 and 5. According to the experiment 1 and experiment 2 were rod shape and they were aggregated to each other. The SEM image from experiment 3 was cylindrical shape.The morphology of image of soda ash from optimum condition was shown in Fig.6. It was more aggregate and fine than experiment 1, experiment 2 and 3. According to the SEM images , the shapes of soda ash samples were generally in they were formed as crystalline structure. Some of them were aggregated and some were scattered. Figure.3. SEM image of Soda Ash from Experiment 1 Figure.4. SEM image of Soda Ash from Experiment 2 Optimal Condition Experiment Experiment Experiment Standard soda ash Optimum Condition Experiment Experiment Experiment International Journal of Trend in Scientific Research and Development (IJTSRD) @ www.ijtsrd.com 27841 | Volume – 3 | Issue – 5 | July - August 2019 hest intensities peaks from optimum condition was occurred at 2 𝜃( (29.953). According to the XRD patterns, the 2. XRD patterns of Synthetic Soda Ash Scanning Electron Microscopy (SEM) In this study ,the morphology of synthetic soda ash were by Sacnning Electron Microscopy (SEM). The SEM images of soda ash from expermient 1, 2 and 3 were shown in Fig. 3,4 and 5. According to the SEM images, experiment 1 and experiment 2 were rod shape and they were aggregated to each other. The SEM image from experiment 3 was cylindrical shape.The morphology of SEM image of soda ash from optimum condition was shown in more aggregate and fine than experiment 1, experiment 2 and 3. According to the SEM images , the nerally in rod shape and structure. Some of them were aggregated and some were scattered. Figure.3. SEM image of Soda Ash from Experiment 1 Figure.4. SEM image of Soda Ash from Experiment 2 Figure. 5. SEM image of Soda Ash from Experiment 3 Figure.6 SEM image of Soda Ash from Optimum Condition 3. Energy Dipersive X-ray Fluorescence (EDXRF) Quantitative results of soda ash were analyzed by using Energy DipersiveX-rays Fluorescence(EDXRF).Accordingto the EDXRF results, carbon percent from experiment (1) , experiment (2) and experiment (3) were 92.64% , 93.73% and 92.53 % respectively . Sodium percent from experiment (1), experiment (2) and experiment (3) were 7.07 % , 6.08% and 7.27% respectively. According to t results, the optimnum condition ofsoda ashwas Fourier Transform Infread Spetroscopy (FTIR). 4. Fourier Transform Infrared Spectroscopy (FTIR) The optimum conditionofsoda ashpepared by Box experimental design was analyzed by Fourier Transform Infrared Spectroscopy .The spectra was recorded in the range (500- 4000 cm -1) . According to the infrared spectrum of soda ash , the stretching bonds of (O approximately 3500 cm-1 and 3000 cm have been attributed to hydroxyl group.The stretchingbond of (C-O) was occurred at 1454.38 cm of (C-CL) was occurred at 858.38 cm impurities in the sample.The infrared spectrum of soda ash from optimum condition is nearly the same as soda ash [11]. Wavelength (cm Figure.7. Infrared Spectrum of Standard Soda Ash[1 ptimal Condition Experiment - 3 Experiment - 2 Experiment -1 soda ash Optimum Condition Experiment -3 Experiment -2 xperiment -1 T % 85 www.ijtsrd.com eISSN: 2456-6470 August 2019 Page 1808 Soda Ash from Experiment 3 SEM image of Soda Ash from Optimum Condition ray Fluorescence (EDXRF) Quantitative results of soda ash were analyzed by using rays Fluorescence(EDXRF).Accordingto results, carbon percent from experiment (1) , experiment (2) and experiment (3) were 92.64% , 93.73% and 92.53 % respectively . Sodium percent from experiment (1), experiment (2) and experiment (3) were 7.07 % , 6.08% and 7.27% respectively. According to the experimental results, the optimnum condition ofsoda ashwas analyzedby Fourier Transform Infread Spetroscopy (FTIR). Fourier Transform Infrared Spectroscopy (FTIR) soda ashpepared by Box-Behnken experimental design was analyzed by Fourier Transform Infrared Spectroscopy .The spectra was recorded in the ) . According to the infrared spectrum of soda ash , the stretching bonds of (O-H) were observed at and 3000 cm-1respectively and have been attributed to hydroxyl group.The stretchingbond occurred at 1454.38 cm -1 .The stretching bond occurred at 858.38 cm-1 that is due to the ample.The infrared spectrum of soda ash from optimum condition is nearly the same as the standard Wavelength (cm-1) Figure.7. Infrared Spectrum of Standard Soda Ash[1
  • 5. International Journal of Trend in Scientific Research and Development (IJTSRD) @ www.ijtsrd.com eISSN: 2456-6470 @ IJTSRD | Unique Paper ID – IJTSRD27841 | Volume – 3 | Issue – 5 | July - August 2019 Page 1809 Figure.8. Infrared Spectrum of Soda Ash from Optimum Condition E. Application of Soda Ash According to the analytical results of the synthetic soda ash , it was confirmed as soda ash. It was applied in water softening process for removal of total harhness of water. Water sample was taken from the laboratory of Chemical Engineering Department from West YangonTechnological University Campus, Hlaing Tharyar Township, Yangon Region.Water analysis was carried out by APHA standard methods. The charaterization of raw water was shown in Table(VI). TABLE(VI).Characterization of Raw Water No Specifications Value 1 Total Hardness(ppm) 255 2 Total Alkalinity(ppm) 85 3 Calcium(ppm) 47 4 Magnesium(ppm) 4.37 5 Sulfate(ppm) 43.1 6 Chloride(ppm) 400 7 Iron(ppm) 28 8 pH 7.9 F. Water Softening 1. Precipitatives Softening Precipitative softening uses lime (Ca(OH)2) and soda ash (Na2CO3) to remove calcium and magnesium ions from solution. Lime added to water reacts first with free carbon dioxide forming a calcium carbonate precipitate .The lime reacts with free carbon dioxide forming a calcium bicarbonate present . In both of these equation one equivalent of lime reacts with free carbon dioxide forming a calcium carbonate precipitate. The lime reacts with any calcium bicarbonate present. In both of these equations,one equivalent of lime combines with one equivalent of either CO2 or Ca(HCO3)2 . CO2 + Ca(OH)2 CaCO3 + H2O (4) [4] Ca(HCO3)2 + Ca(OH)2 2CaCO3 + 2H2O (5) [4] Since magnesium precipitates as Mg(OH)2 Mg (HCO3)2 + Ca(OH)2 MgCO3 + CaCO3 + 2H2O (6) [4] MgCO3 + Ca (OH)2 Mg (OH)2 + CaCO3 (7) [4] MgSO4 + Ca(OH)2 CaSO4 + Mg(OH) (8) [4] Lime- soda softening Removal of Carbonate hardness with lime Ca2+ + 2HCO3 - + Ca (OH)2 2CaCO3 + 2H2O (9) [13] Mg2+ + 2HCO3 + 2Ca(OH)2 2CaCO3 + Mg(OH)2 + H2O(10) [13] Removal of non-carbonate hardness with soda ash and lime Ca2+ + 2Cl- +Na2CO3 CaCO3 + 2Na+ +2Cl- (11) [13] Ca2+ + SO4 2- + Na2CO3 CaCO3 + 2Na+ + SO4 2- (12) [13] Mg2+ + 2Cl- + Ca(OH)2 Mg(OH)2 + Ca2++ 2Cl- (13) [13] Mg2++ SO4 2-+ Ca(OH) Mg(OH)2 +Ca2++ SO4 2- (14)[13] Recarbonation for pH Control CO3 2- + CO2+ H2O 2HCO2 3 - (15) [13] In this research , water soft ening process was carriedout by various dosage of lime and soda ash.Experiment (I)was carried out by single-stage lime-softening process. Experiment (II) was carried out by synthesized soda ash. Experiment (III) was carried out by watersoftening byusing both lime and synthesized soda ash. Experiment (IV) was carried out by water softening by using both lime and commercial soda ash. 1. Procedure of Water Softening with Lime In experiment I , raw water (100) ml was taken to treat with 10 % lime solutuion (Ca(OH)2). And then , it was stirred by magnetic stirrer with 500 rpm. After that it was settled for 10 min. The lime treated water was passed throughthefilter paper and pH was measured before and after filtration. According to this experiment, when the lime dosage was increased, the pH of water was increased from initial condition to pH 9. On the other hand, total hardness was decreased from initial condition of 255 ppmto229,200,242 ppm respectively. According to the experimentalresults,the optimum condition was observed at0.3mloflimefor100ml of sample water. The effect of various dosage of lime vs total hardness and pH was shown in Figure 8. Figure.8. Effect ot of Total Hardness and pH with various dosage of Lime Solution
  • 6. International Journal of Trend in Scientific Research and Development (IJTSRD) @ www.ijtsrd.com eISSN: 2456-6470 @ IJTSRD | Unique Paper ID – IJTSRD27841 | Volume – 3 | Issue – 5 | July - August 2019 Page 1810 According to this graph, whenlimedosagewas increased, pH was steadily increased. However, lime dosage was exceeded over the required level, hardness of water was returned to increase . According to this graph , only lime solutioncannot reduced the total hardness significantly. 2. Procedure of Water Softening Process With Synthesized Soda Ash In experiment (II) , raw water (100) ml was taken to treat with 5 % synthesized soda ash solution . And then it was stirred by magnetic stirrer with 500 rpm. After that , it was settled for 10 min and passed through a filter paper. The soda ash treated water was analyzed by EDTA titration method to know the removal efficiency of total hardness. According to the experimental results , hardness of water was effected by various dosage of soda ash.When thedosage was increased , the pH of water was significantly increased. So , the hardness and pH of water were inversely proportional according to the dosage of soda ash. However, the dosage of synthesized soda ash was exceeded over the required level , hardness level of water was increased significantly. The effect of synthesized soda ash vs total hardness and pH was shown in Figure.9. Figure.9. Effect of Total Hardness and pH with Various Dosage of Synthesized Soda Ash Solution According this graph, pH level was sharply raised when the dosage was increased. The hardness of water was significantly decreased from initial condition of 255 ppm to 171 ppm. However, hardness level was returned to increase when the dosage was increased. 3. Procedure of Water Softening Using Both Lime and Synthesized Soda Ash In experiment (III ) , water sample was treatedby using both lime and synthesized soda ash. According to the lime process, 0.3 ml of lime was taken as optimum condition because which removed the hardness than other dosage. According to the lime dosage, the pH level of water was raised; the bicarbonates ions were converted to carbonate concentration. Due to the increase in carbonate concentration, precipitates of calcium carbonate were formed. The remaining calcium cannot be removed by simple adjustment of pH. So, soda ash solution was addedby varying the dosage to precipitates the remaining calcium. In lime-soda treatment, the pH level was raised by addition of lime while sodium carbonate was added to reduce residual carbonate hardness. The treated water was passed through the filter paper, and then it was analyzed by EDTA titration method. According to the experiment, lime and various dosage of synthesized soda ash was effectively reduced the water hardness. Maximum removal percent of hardness of water was observed at 0.3 ml of lime and 2 ml of synthesized soda ash. The effect of both lime and soda ash dosage vs pH and total hardness was shown in Fig. 10. Figur.10. Effectof Lime-Soda Dosage by Synthesized Soda Ash According to this graph , hardness of waterwas dramatically decreased but pH of water was increased. When the dosage of was increased over the required level, the hardnesslevel of water was slightly increased. 4. Procedure of Water Softening Using Both Lime and Commercial Soda Ash In experiment IV, lime-soda softening process was carried out using the commercial grade soda ash to reduce the hardness of water. The procedure was the same as using the lime and various synthesized soda ash. According to the results, water softening by using both lime and commercial soda ash dosage effectively reduced the water hardness. The maximumremoval ofhardnessofwater was observed at 0.3 ml of lime and 2ml of commercial soda ash. The effect of lime and soda ash dosage on pH and total hardness was shown in Figure 11. Figur11.Effect of lime and various dosage of commercial soda ash According to this graph, hardness of water was dramatically decreased but pH of water was increased. When the dosage was increased over the required level, the hardness level of water was slightly increased.
  • 7. International Journal of Trend in Scientific Research and Development (IJTSRD) @ www.ijtsrd.com eISSN: 2456-6470 @ IJTSRD | Unique Paper ID – IJTSRD27841 | Volume – 3 | Issue – 5 | July - August 2019 Page 1811 5. Jar Testing Firstly, one liter of sample water was taken and added to each of the beakers of gang-mixersystem.Themixers in each beaker were allowed to set a mixing rate of 150 rpm. Next, 5% of commercial grade sodium carbonate solution was added into the first beaker. And then, 5% of synthesized soda ash solution was added into the second beaker and allowed to mix with 150 rpm. According to the lime-soda softening process, the optimum condition of 3 ml of lime solution was added into the third and fourth beakers. After 10 minutes, the beakers were allowed to settle. Following the settling period, the samples were collected from each beaker and filtered. The pH levels were measured for adjusting the optimum range. After that, 5% synthesized soda ash solution was added into lime treated water by varying dosage. The mixers in each beaker were allowed to set up the 150 rpm. After 10 minutes, the beakers were allowed to settle for 10 minutes. After settling, the samples were filtered. The pH was measured before and after filtration. And then it was passed through by carbon dioxide gas to obtain the acceptable pH range of (6.5- 8.5). Finally, the treated waters were measured pH and total hardness. According to the jar testing results, lime-soda softening process was more effectively reduced the hardness of water than only synthesized soda ash dosage. Water softening by using both synthesized soda ash dosage and lime is more effective. According to the lime-soda softening process, the optimum condition for one liter water was observed at 3 ml of lime and 20 ml of synthesized soda ash. And then, the treated water from the optimum condition was passed through by carbon dioxide to obtain acceptable pH range of 6.5 ~ 8.5. Finally, it was measured to total hardness, total alkalinity, calcium, magnesium, sulfate, chloride and iron. The result of treated water by jar test was shown in Table VII. The Specifications of treated water was shown in Table VIII. Table VII. JAR Testing Results Run No Volume of Sample Water (ml) 10% lime Solution 5%Soda Ash Solution (ml) Settling Tim(min) pH Total Hardness Hardness Removal %Synthesized Commercial 1 1000 - 20 - 10 9 185 27.45 2 1000 - - 20 10 9 175 31.72 3 1000 3 20 - 10 9.5 24 90.59 4 1000 3 10 -- 10 9 26 89.80 TABLE VIII SPECIFICATION OF TREATED WATER No Specifications Raw Water Value Treated Water Value 1 Total Hardness(ppm) 255 24 2 Total Alkalinity (ppm) 85 240 3 Calcium(ppm) 47 9.02 4 Magnesium(ppm) 4.37 0.2 5 Sulfate(ppm) 43.1 45.2 6 Chloride(ppm) 400 370 7 Iron(ppm) 28 < 8 pH 7.9 6.5 According to the experimental results, the concentration of raw water and the treated water were different. Lime-soda softening process was reduced the hardness from initial concentration of 255 pm to 24 ppm. However, the total alkalinity was increased from initial condition of 85 ppm to 240 ppm according to the lime dosage. Calcium, magnesium and iron were dramatically reduced from initial concentrations because of lime and soda ash dosage. Sulfate was slightly increased from initial concentration of 43.1 to 45.2 ppm. Chloride was slightly reduced from 400 ppm to 370 according to lime-soda dosage. Before carbonation, pH of treated water is 9.5; it was reduced to pH 6.5 by passing carbon dioxide gas. It was within the acceptable level. The initial pH of raw water is 7.9.The final pH of treated water was 6.5. IV. CONCLUSIONS In this study, the soda ash is prepared synthetically by Solvay process by the use of Box-Behnken experimental design. The maximum yield percent of 19.882% was obtained with the reaction salt to ammonium hydroxide to carbon dioxide ratio of 1:3:6.8 during reaction time 90 minutes. According to the XRD patterns, SEM images and FTIR result, the optimum condition which prepared by Box- Behnken experimental design is said tosoda ashand applied in water softening process. Water softening was carried out by lime softening,softening by synthesized soda ash, softening by commercial soda ash and lime-soda softening process. According to the experimental results, lime softening process cannot adequately reduce the hardness level. Softening by synthesized and commercial soda ash can reduce the hardness level of water. However, the lime-soda process can effectively reduce the hardness level of water. The initial characteristics of raw water is total hardness of 255 ppm, total alkalinity of 85 ppm, calcium of 47 ppm , magnesium of 4.37 ppm , sulfate of 43.1 ppm , chloride of 400 ppm , iron of 28 ppm. The initial pH is 7.9. After lime-soda treatment, thetotalhardness of 24, total alkalinity of 240, Calcium of 9.02, Magnesium of 0.2, Sulfate of 45.2%, Chloride of 270, Iron of < 0.1 and pH of 6.5 are obtained.
  • 8. International Journal of Trend in Scientific Research and Development (IJTSRD) @ www.ijtsrd.com eISSN: 2456-6470 @ IJTSRD | Unique Paper ID – IJTSRD27841 | Volume – 3 | Issue – 5 | July - August 2019 Page 1812 ACKNOWLEDGEMENT The author would like to express her thankstoallprofessors and all lecturers of Chemical Ennginering Department,West Yangon Technological University for giving the opportunity to carry out this reseasrch. And also the author is deeply gratitude to professors for their kind advice and systematic guidance . Finally, the author is particularly indebted to Chairman of Green Myanmar Environmental Services for financial support and lab facility for preparing this research. RFERENCES [1] T. Madima , “ Manufcturing of Synthetic Sol da Ash,” M.S.c thesis,University of the Cape, South Africa, Feb.2009 [2] K..E McCaleb , TheBiography of a Chemical Economic Handbook Report ,Chemical Information Services, Stanford Research Institute, Melno- Park ,Calif.94025 , Nov. 1971 [3] R. H. MyersandD. C. Montgomery, “Response Surface Methodoloy,” 3rd Edition,2008 [4] Aung Myint Soe , “ ChT-2024, Introduction to Chemical Technology” Lecture Note, 2003, Department ot Chemical Engineering , Yangon Technological University [5] Housecroft, C.E and Sharpe, A.G. 2004. Inorganic Chemistry. 2nd edition. Prentice Hall. P187 [6] Air Products and Chemicals (APC), Inc,2009 . “Carbon Dioxide”Product Stewardship Summary [7] M.C.RAND, A.E.GREENBERG, M. J. TARAS , “Standards Methods For the Examination of Water and Waste Water,” 14 th edition [8] Dr. G. W.Latimer, Jr, “Officials Methods of Analysis ofAOAC International , ” 20th edition, 2016 [9] ESEPA- European Soda Ash Procedure Association , “Process BREF For Soda Ash” ,March 2004. [10] R.A.Meyers (Ed.), Encylopedia of Analytical Chemistry, pp.10815-10837, 2000 [11] Anonymous ,”Sodium Carbonate, Database of ART- FT_IR spectra of various materials< lisa_Chem_ut.ee>IR_spectra>paint> paint>fillers [12] Dipa Dey,Amanda Herzog, Vidya Srinivaszn,“Chemical Precpitation: “Water Softening” , ENE806, May 2 ,2007