Analysis of the effect of flow rate, packing size and materials

on the overall performance of the absorption process in a

packed absorption column.
1
Ameerul Afiq, 2Arina Hazirah, 3Mohd Asraf, and 4Yuweta
1,2,3,4
Chemical Engineering Section

Universiti Kuala Lumpur Malaysian Institute of Chemical and Bioengineering Technology

1988 Bandar Vendor, Taboh Naning, 78000 Alor Gajah, Melaka, MALAYSIA.
1
E-mail: [email protected] 2E-mail: [email protected]
3
E-mail: [email protected] 4E-mail: [email protected]

Abstract

Packed columns are commonly used in chemical industry to remove volatile substances from a
liquid or to absorb a gas from a mixture of gases. Usually, the columns use countercurrent flow,
in which gas flows upward, and liquid flow downward. Packings are filled inside the column to
provide large contact area for mass transfer between gas and liquid. There is a need to find the
optimum condition for the operation of an absorption column in order to increase the absorption
efficiency of the process, while at the same time reduce the energy requirement and ensure
optimized mass transfer. Several factors need to be taken into consideration before this
optimization can be done. In this open-ended experiment, we were tasked to run an absorption
process using a Packed Absorption column and to analyze the effect of the different flow rate that
can affect the overall performance of the absorption process. Not only that, we were also tasked
to investigate the effects of different types and sizes of the packing materials on the efficiency of
CO2 removal. This analysis is done using direct titration between HCL and mixture of NaOH and
CO2 mixture from the column to find the unreacted NaOH.

Keywords: absorption column, packing material, packing size, percentage removal, CO2 removal

Highlights

• Lower flow rate will lead to a better percentage removal of CO 2.

• Big sized packing material will lead to a better percentage removal of CO2 as it will have
a larger contact area for carbon dioxide and water, hence facilitating the absorption
process.
• Ceramic material will have a better CO2 removal percentage compared to glass material.
 1. Introduction/Theory vapour gas flow across the column cross-
section.
This study aims to analyze the effect of flow
rate, packing size and packing material
towards the percentage removal of CO2 and
Packing can be generally divided into two
towards the overall performance of the
types, which are regular geometry packings
absorption process.
and random packings. Regular geometry
According to IUPAC (Absorption, 2019), packings have regular geometry such as
absorption is defined as the process of a stacked grids and structured packings. On
single material, absorbate, retained by the other hand, random packings consist of
another material, absorbent. Absorption rings, saddles and proprietary shapes, which
process can be either physical or chemical, are dumped into the column and assumed a
depending if any chemical reaction occurs random arrangement. Random packings are
between the absorbate and absorbent, in more commonly used in the process industry
which atoms, molecules or ions penetrate (Sinott, Richardson & Coulson, 2013). This
the bulk phase of either liquid or solid experiment will also utilize random packings
material and are distributed throughout the in the separation process.
whole volume of absorbent. If no significant
chemical reaction occurs between the
absorbate and absorbent, the process is There is a need to know the maximum gas
referred to as physical absorption. In the flow rate that can be used. This is because
experiment, gas mixtures are pumped from higher gas flow rate will lead to a greater
the bottom while water are pumped from the resistance felt by the liquid and a higher
top, in a counter-current manner. This pressure drop across the packing materials.
process is known as gas absorption or When the gas flow rate becomes too much,
scrubbing, due to the reason that the contact a condition called flooding occurs where the
between gas mixture and liquid for the liquid will fill the entire column and will lead
purpose of dissolving components of the gas to difficulties in carrying out the operation.
into the liquid. The high pressure then will damage the
packings in the column. To prevent this, the
gas flow rate should be ½ of the flooding
Packing materials in packed absorption velocity. Otherwise, a specified pressure
column plays a huge part in the absorption drop condition can be set which will be well
process as they facilitate the process of below the pressure drop in which flooding
absorption through their large contact area would occur (“Column Diameter and
which enables the two phases to be in Pressure Drop”, 2019).
contact. These packing materials are usually
made from either plastics, ceramics or
metals. According to Sinott, Richardson & Generally, the packing size depends on the
Coulson (2013), good packing materials size of the column itself. However, the
should provide a large contact area between general rule is that the packing size should
the gas and liquid, have low resistance to gas not exceed 50 mm as smaller packing cost
flow, promote uniform liquid distribution on more compared to larger packing. Besides
the packing surface, and promote uniform that, the usage of large packing in a small
 column will cause poor liquid distribution with sodium hydroxide to for sodium
(Sinott, Richardson & Coulson, 2013). The hydrogen carbonate, which are neutral, thus
recommended packing sizes according to completing the reaction.
the column diameter is shown in Table 1.

𝑁𝑎𝑂𝐻 (𝑎𝑞) → 𝑁𝑎+ + 𝑂𝐻− (3)

Table 1: Packing size according to column 𝐻2𝐶𝑂3 (𝑎𝑞) + 𝑁𝑎𝑂𝐻 (𝑎𝑞) → 𝑁𝑎𝐻𝐶𝑂3 (𝑎𝑞) +
diameter. (Source: Sinott, Richardson & 𝐻2𝑂(𝑎𝑞) (4)
Coulson, 2013)

Column diameter Packing size to be used

When determining the efficiency of water in
< 0.3 m (1 ft) < 25 mm (1 in.) removing carbon dioxide content in air by
using a packed bed reactor, four factors
0.3 to 0.9 m (1 to 3 ft) 25 to 38 mm (1 to 1.5 in.) influencing the rate of absorption have to be
> 0.9 m 50 to 75 mm (2 to 3 in.) taken into consideration; flowrate of water,
flowrate of gas, size of packing material and
material of construction of the packing
There are many parameters that need to be material.
considered before designing a packed
absorption column to obtain maximum
efficiency of gas absorption and to prevent As for the effect of water flowrate and gas
flooding problem from occurring. flowrate to the absorption of carbon dioxide
into water, it should be fairly straightforward.
When carbon dioxide is absorbed into the Since physical absorption involve an
liquid water, it reacts with the liquid water to absorbate to be absorbed by absorbent, an
form dihydrogen carbonate (carbonic acid), increase in water (absorbent) flowrate and
which dissociates further to for aqueous decrease in gas (absorbate) flowrate should
hydrogen and aqueous hydrogen carbonate result in increase of absorption of carbon
ions. dioxide into water, proven by the findings of
Tan, Shariff, Lau, & Bustam (2012).

𝐶𝑂2(𝑔)+ 𝐻2𝑂 (𝑙)→ 𝐻2𝐶𝑂3 (𝑎𝑞) (1)

𝐻2𝐶𝑂3 (𝑎𝑞)→ 𝐻+ + 𝐻𝐶𝑂−3 (2)

In order to determine the amount of carbon

dioxide being absorbed into the water,
neutralization of carbonic acid is done since
the amount of carbonic acid formed id
proportional to the amount of carbon dioxide
absorbed by the water. Thus, sodium
hydroxide is used, which are readily
dissociates in water into sodium ion and
hydroxide ion. The carbonic acid then reacts
 According to Arachchige & Melaaen (2012),
the effect of packing material and packing
material size on carbon dioxide absorption
are influenced by factors including specific
surface area, surface area spread uniformity,
void space per unit column volume and
friction. In general, maximum specific
surface area in uniform manner with
maximum void space per unit column volume
and minimal friction will result in the greatest
removal of carbon dioxide in gas mixture.
This is due to the result of improved vapor-
liquid contact from increased surface area
and uniformity of packing material. By
maximizing the void space per unit column
Figure 1: Effect of gas flowrate to CO 2 volume and minimizing friction, the gas faces
concentration (Tan, Shariff, Lau, & Bustam, minimal resistance when going up the flow.
2012).
 FCV 2, and V1 were opened to allow the air
and CO2 to enter the column and gave the
2. Procedure
required air flowrate as indicated by FI1 and
2.1 Start up FI2, and V11 will be opened. The absorption
process was let to stable for 10 minutes to
Firstly, recirculation vessel was filled up with attain steady state. After 10 minutes,
water for about half of the vessel. Valves samples will be collected at valve V12 for half
FCV1, FCV2, FCV3, FCV4, V7, V12 and V13 an hour to analyze the removal of CO2.
were ensured to be closed. The column to be
operated was chosen and the valves were For Column 2, the power switch of
adjusted according to the table below. The recirculation pump is turned on. All valves
manometer reading was set to zero, and the were ensured to be closed except for V5, V7,
selector valve switch, SV1 must be V9, and V13. Next, FCV4 was slowly opened
connected to the chosen column. and was adjusted to obtain the flowrate of 5
L/min as indicated by FI3. After that, FCV1,
Table 2: Valve opening & column relation FCV 2, and V2 were opened to allow the air
Column Column Column and CO2 to enter the column and gave the
1 2 3 required air flowrate as indicated by FI1 and
V1 O X X FI2, and V11 will be opened. The absorption
V2 X O X process was let to stable for 10 minutes to
V3 X X O attain steady state. After 10 minutes,
V4 O X X samples will be collected at valve V12 for half
an hour to analyze the removal of CO2.
V5 X O X
V6 X X O
V7 O O O
2.3 Comparison of Material Type: Column 2
V8 O X X
vs Column 3
V9 X O X
V10 X X O For Column 2, the same data was taken from
SV1 O O O previous step at column 2. For Column 3, the
power switch of recirculation pump is turned
on. All valves were ensured to be closed
O – Open
except for V6, V7, V10, and V13. Next, FCV4
X – Closed was slowly opened and was adjusted to
obtain the flowrate of 5 L/min as indicated by
FI3. After that, FCV1, FCV 2, and V3 were
2.2 Comparison of Material Size: Column 1 opened to allow the air and CO 2 to enter the
vs Column 2 column and gave the required air flowrate as
indicated by FI1 and FI2, and V11 will be
For Column 1, the power switch of opened. The absorption process was let to
recirculation pump is turned on. All valves stable for 10 minutes to attain steady state.
were ensured to be closed except for V4, V7, After 10 minutes, samples will be collected at
V8, and V13. Next, FCV4 was slowly opened valve V12 for half an hour to analyze the
and was adjusted to obtain the flowrate of 5 removal of CO2.
L/min as indicated by FI3. After that, FCV1,
2.4 Analysis of Carbon Dioxide in Water then tabulated, and the experiment was
Sample repeated with samples from different
columns.
Every 10 minutes, 10mL sample from the
outlet valve was taken. After that, 30mL of
0.01 M NaOH solution was added to the
2.5 Shut Down
sample. The volume of NaOH was in excess
to allow all CO2 had reacted with NaOH in the The CO2 supply and the compressed air
mixture. Next, a few drops of indicator supply at valve SG & CA is slowly closed.
(phenolphthalein) was dropped to the Next, the power switch of recirculation pump
solution. The mixture was then titrated with is turned off. After that, the air supply and
0.01 M HCl solution to obtain the amount of CO2 supply were also turned off. Valve V11
unreacted NaOH. The titration process was will be opened to allow fresh water to enter
repeated every 10 minutes with fresh the column for a few minutes to drain off the
samples until 30 minutes. The results were water.
3. Result
Volume of NaOH = 30mL
Volume of CO2 in sample = 10mL

Table 3: Volume of HCL at air flowrate 20 L/min and 40 L/min at Colum 1 (small glass)

Air flowrate Time (min) Water flowrate Volume of HCL (mL)

(L/min) (L/min)

10 1 21.90
20
20 3 22.50

30 5 23.40

10 1 17.90

20 3 18.80
40
30 5 21.15

Table 4: Volume of HCL at air flowrate of 40 L/min at Column 2

Time, t (min) Water flowrate (L/min) Volume of HCL (mL)

10 1 24.00
20 3 22.50
30 5 22.10

Table 5: Volume of HCL at air flowrate of 40 L/min at Column 3

Time, t (min) Water flowrate (L/min) Volume of HCL (mL)
10 1 24.35
20 3 23.25
30 5 22.30
Table 6: Concentration of CO2 in inlet and outlet and percentage removal of CO2 at air
flow rate at 20 L/min at column 1
Concentration Concentration Concentration Percentage
Time, t (min) of CO2 inlet of CO2 outlet of CO2 in water removal of
(mol/L) (mol/L) (mol/L) CO2 (%)

10 0.045 4.05 ×10-3 0.04095 91.00

20 0.045 3.75×10-3 0.04125 91.67

30 0.045 3.25×10-3 0.04175 92.78

Table 7: Concentration of CO2 in inlet and outlet and percentage removal of CO2 at air
flow rate at 40 L/min at column 1
Concentration Concentration Concentration Percentage
Time, t (min) of CO2 inlet of CO2 outlet of CO2 in water removal of
(mol/L) (mol/L) (mol/L) CO2 (%)

10 0.045 6.05 ×10-3 0.03895 86.56

20 0.045 5.60×10-3 0.03940 87.56

30 0.045 4.43×10-3 0.04057 90.16

Table 8: Concentration of CO2 in, inlet and outlet and percentage removal of CO2 at air
flow rate at 40 L/min at column 2
Concentration Concentration Concentration Percentage
Time, t (min) of CO2 inlet of CO2 outlet of CO2 in water removal of
(mol/L) (mol/L) (mol/L) CO2 (%)

10 0.045 3.00 ×10-3 0.04200 93.30

20 0.045 3.75×10-3 0.04125 91.67

30 0.045 3.95×10-3 0.04105 91.22
 Table 9: Concentration of CO2 in, inlet and outlet and percentage removal of CO 2 at air
flow rate at 40 L/min at column 3
Concentration Concentration Concentration Percentage
Time, t (min) of CO2 inlet of CO2 outlet of CO2 in water removal of
(mol/L) (mol/L) (mol/L) CO2 (%)

10 0.045 2.825×10-3 0.042175 93.72

20 0.045 3.37510-3 0.041625 92.50

30 0.045 3.850×10-3 0.041150 91.44

Table 10: Average percentage removal of CO2

Column Percentage removal CO2 (%)
1 at 20 mL/min 91.82
1 at 40 mL/min 88.09
2 at 40 mL/min 92.06
3 at 40 mL/min 92.35
 94

Percenntage of CO2 removal (%)

93

92

91

90
20 L/min
89
40 L/min
88

87

86
0 5 10 15 20 25 30 35
Time (min)

Figure 2: Percentage removal of CO2 (%) against time (min) for Column 1 at air flowrate of
20 L/min and 40 L/min

94

93
Percentage of CO2 removal (%)

92

91

90
Column 1
89
Column 2
88

87

86
0 5 10 15 20 25 30 35
Time (min)

Figure 3: Percentage removal of CO2 (%) against time (min) for Column 1 and Column 2 at
flowrate of 40 L/min
 94

Percentage of CO2 removal (%)

93.5

93

92.5
Column 2

92 Column 3

91.5

91
0 5 10 15 20 25 30 35
Time (min)

Figure 4: Percentage removal of CO2 (%) against time (min) for Column 2 and Column 3 at
flowrate of 40 L/min
4. Discussion phenolphthalein. The sample is then directly
titrated with 0.01M hydrochloric acid. The
Throughout this experiment, the
samples were titrated with hydrochloric acid
objective was to study how the different
until an observation of first pale pink
flowrate of gas and liquid effect the rate of
presents.
absorption of carbon dioxide. Besides, this
experiment was carried out to study how the According to Table 3, the volume of
packing material of different material and the titrated hydrochloric acid needed to
size effect the rate of absorption of carbon obtain the pale pink observation are
dioxide. There were three types of packed recorded. The hydrochloric acid titration
column being used to conduct the causes the carbon dioxide in the solution to
experiment and which were Column 1 (small react with the sodium hydroxide to form
sized glass material), Column 2 (big sized sodium bicarbonate. The phenolphthalein
glass material) and Column 3 (ceramic indicator then determines the amount of
material). Within the objectives, the unreacted sodium hydroxide with carbon
experiment is separated into two parts; the dioxide in the sample mixture. In flow rate at
first part, the experiment is conducted using 20 L/min, the hydrochloric acid volume
the instrument of packed column gas increased with the time when the flowrate of
absorption. Meanwhile, another experiment water was increased of 1,3 and 5 L/min; until
focused on the chemical preparations which the experiment reaches the time at 30th
used for the sample analysis from the first minute. There were three readings taken due
experiment, using direct titration. The to study the differences of 2mL between the
instrument of packed column gas absorption flowrate of water. The highest volume of
was stable by constant water flow rate by 10 HCL for the flow rate 20 L/min was 23.4 mL
minutes. This was to ensure that the surface at 30 minutes while the lowest volume was
of glass was wet by the water to produce gas 21.9 ml at the beginning of zero minute.
carbon dioxide. Overall, this experiment was Likewise, to the flow rate at 40 L/min the
conducted by the changes of variable which volume of HCL needed increase within time.
are at air flow rate 20 L/min and 40 L/min at Based on the Figure 2, when compared
Column 1 while for Column 2 and 3 the air between the two flowrates, was concluded
flowrate was at 40 L/min. Every 10 minutes, that the percentage of carbon dioxide
the sample was taken for the measurement removal at the flowrate of 20 L/min was
of the concentration of carbon dioxide. Each higher compared to flowrate of 40 L/min
sample were added with 30 mL of 0.01 M which was the average of carbon dioxide
sodium hydroxide and a few drops of removed at 20 L/min is 91.82%.
 The Column 1 and 2 were studied on between the volume of hydrochloric acid as
how the size of the packing material affect per Table 4 and 5 , the values were not
the absorption of carbon dioxide at flowrate showed in big range of differences between
of 40 L/min. As shown in Table 4 and 5, at the values were obtained from Column 2 and
the flowrate or 40 L/min, the percentage of 3. Based on Figure 4, the trendline of Column
carbon dioxide removed at Column 1 2 and 3 were individually decreased with time
increased with time, while at the Column 2 increased but according to Table 10, the
the percentage of carbon dioxide removal percentage removal of carbon dioxide at
decreased with time. Based on Figure 3, it Column 3 was 92.35% while Column 2 was
was shown that the trendline of Column 2 92.06% which showed that at Column 3
was being decreased with time increased which used ceramic material absorbed more
compared to the Column 1 at the flowrate of carbon dioxide compared to Column 2 which
40 L/min. however, based on Table 10, was glass material. This is due to the friction
average percentage of carbon dioxide property of material. The ceramic material
removal was higher at Column 2 compared has less friction compared to the glass
to Column 1.This is because the big sized material.
packing material inside of Column 2 has
There were three main factors that
larger contact area for the absorption
affected the percentage removal of CO2,
process to occur compared to the smaller
which are the interfacial between gas phase
material inside Column 1, which means that
and liquid phase, the resistance in the gas
Column 2 has the capacity of absorbing
phase and the resistance in the liquid phase.
higher amount of carbon dioxide compared
In the process of absorption, the total gas
to Column 1.
flow rate is constantly changing due to CO2
Furthermore, the experiment was absorption into water solution. According to
conducted on comparing the types of Yeh & Pennline (2001), the mass transfer
material of packed Column 2 with the packed resistance of the gas phase will decrease
Column 3 which the Column 2 was packed with the increasing CO2 partial pressure
with glass material while Column 3 was which is according to two-film theory.
packed with ceramic material at constant Basically, an increase in the CO 2 partial
flowrate of 40 L/min. According to Table 4, pressure allows more CO2 molecules to
for Column 2, the volume of hydrochloric acid travel from gas bulk to the gas-liquid
used increased with time and likewise interface, which would result in higher mass
happened at Column 3, as proven from transfer performance. In case of the liquid
Table 5. When the values were compared flow rate, it was found that an increase in the
liquid flow rate results in an increase in mass This is because ceramic packing material
transfer coefficient value. This means there has less friction compared to glass material
were more liquid would be spread on the which will then improve the absorption
packing surface and this led to an increasing process. Large packing size is preferred as it
in the interfacial area per unit volume. For the has a larger contact area between the
case of gas flow rate, increase in the gas flow carbon dioxide and water, thus further
rate leads to a higher mass transfer facilitates the absorption process to occur
coefficient value especially when the carbon compared to smaller packing materials.
dioxide concentration is high. This is due to
References
the increase of the wetted surface packing
material for gas-liquid contact increased with Absorption. (2019). Gas Absorption &
Desorption. Retrieved from
the increasing of the liquid flow rate. Thus,
http://www.separationprocesses.com
increasing the efficiency of mass transfer /Absorption/GA_Chp03.htm
process through the absorption column (Yeh
“Absorption (chemistry)” (2019). Retrieved
& Pennline, 2001). from
https://en.wikipedia.org/wiki/Absorpti
From the conducted experiment, on_(chemistry)
several potential errors have been detected
Alex Randomkat e.t al. (2016). Retrieved
that may obstruct the result obtained. Firstly, from https://www.quora.com/How-
any valve or whatnot can be mistakenly does-the-reaction-of-carbon-dioxide-
operated and alas which could affect the gas-with-sodium-hydroxide-and-
water-solution-occur
product. Next, while running the experiment,
Andselisk e.t al. (2017). Reaction between
it can be observed that the gas absorption
NaOH and CO2. Retrieved from
column contained algae in it which it may https://chemistry.stackexchange.co
contaminate the liquid flowing through the m/questions/57288/reaction-
column. between-naoh-and-co2

Arachchige, U. S., & Melaaen, M. C. (2012).

5. Conclusion Selection of Packing Material for Gas
Absorption. European Journal of
The results from this experiment shows that
Scientific Research,87(1), 117-126.
lower flow rate leads to a better overall
“Column Diameter and Pressure Drop”. (n.
performance of the absorption process. On
d.). Column Diameter and Pressure
the other hand, the usage of large packing Drop. Retrieved from
size and ceramic packing material will http://www.separationprocesses.com
/Absorption/GA_Chp04a.htm
increase the efficiency of CO2 removal, as
evident from the result from this experiment.
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0036.html
Yeh, T. J. & Pennline, W. H. (2001, February
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(2013). Chemical Engineering: An Desorption in a Packed Column.
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Tan, L., Shariff, A., Lau, K., & Bustam, M.
10949, Pittsburgh, Pennsylvania
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Appendices

Based on the reaction below:

2NaOH + CO2 → Na2CO3 + H2O

Na2CO3 + HCL → CO2 + H2O+ NaCl

2 moles of NaOH results with 1 mole of CO2

Let x = moles of NaOH added = 0.01V1

V1= volume of NaOH,

V2 = volume of HCL

y = moles of HCl used = 0.01V2

I. Sample of calculation at Flowrate 20 L/min with time at 10 min

1𝐿
𝑉1 = NaOH being added = 30 𝑚𝐿 × = 0.03 L
1000 𝑚𝐿

𝑚1 𝑉1 = 𝑥 = 𝑚𝑁𝑎𝑂𝐻 × 𝑉𝑁𝑎𝑂𝐻

𝑚𝑜𝑙
𝑥 = 0.01 × (0.03 L) = 3×10−4 mol
𝐿

1𝐿
𝑉2 = HCl being used = 21.90 𝑚𝐿 × = 0.0219 L
1000 𝑚𝐿

𝑚2 𝑣2 = 𝑦 = 𝑚𝐻𝐶𝑙 × 𝑣𝐻𝐶𝑙

𝑚𝑜𝑙
y = 0.01 × (0.0219 𝐿) = 2.19×10−4 mol
𝐿

Then:

moles of NaOH reacted = (x-y)

moles of CO2 reacted = 0.5 (x-y)

Hence: Concentration CO2 outlet = 0.5 (x-y)/ (VCO2 sample)

[0.5(3×10−4 mol −2.19×10−4 mol)] 𝑚𝑜𝑙

= 4.05× 10−3
0.01 𝐿 𝐿
 II. Concentration of CO2 inlet

CO2 Inlet stream:

L
2.0 x5 min = 10 L =0.01m3
min

kg
Density of CO2=1.98
m3

mass
=
volume

kg
Mass of CO2 = 1.98 x0.01m 3 = 0.0198 kg
m3

Mol of CO2 =mass CO2 / molar mass CO2

mole
n = 19.8 g = 0.45mole
44 g

n 0.45mol
conc, c = = = 0.045 mol
v 10 L L

CO2 inlet = 0.045 mol

L

III. Concentration of CO2 in water

Formula: concentration of CO2 inlet – concentration of CO2 outlet

𝑚𝑜𝑙 𝑚𝑜𝑙
= 0.045 𝐿
− (4.05 × 10−3 𝐿
)

𝑚𝑜𝑙
= 0.04095 𝐿
IV. Percentage 𝑪𝑶𝟐 removal.

(Concentration of 𝐶𝑂2 in water / Concentration 𝐶𝑂2 inlet) × 100%

0.04095
= 0.045
× 100 %

= 91 %