A.

Title :Chemical Modification of Sulfur

B. Objectives : 1. Learn some types of sulfur modification
2. Study the properties of hydrogen sulfide and H2SO4
C. Liberature Review
Sulfur is one of the essential macro-nutrient crops that contribute to the
improvement of crops by giving hara hara gives directly, indirectly as a soil
improvement especially with high pH and soil increase the efficiency of use of other
essential nutrient particularly nitrogen and phosphorus. Sulphur content on agricultural
land in the region humid and semi humid about 100 to 500 mg kg-1 or 0.01 up to
0.05% S, while on the ground in the tropics is low due to the low content of S content
of organic materials [1].
Sulfur is a non-metal element multivalen, no taste and no smell. The large
number of valence sulfur (S2-up S6 +) allows sulfur participates in a variety of
biochemical and geochemical processes. In the periodic table, element S is located in
The 3rd Period VIA (or the 16) together with the elements oxygen (O), selenium (S),
tellurium (Te), and polonium (Po) and is referred to as the same group, from Greece
(Chalcos = seed; gen =-forming). So the same group including sulfur was an element
of forming seeds.
In nature, the sulphur everywhere and the numbers are very abundant, even
widespread on Earth and the solar system. Sulfur is the eighth most abundant
element and is present in the largest concentration of silicate layers on Earth
approximately 250 ppm. They can be found as a sulfide mineral in the Earth's mantle,
as sulfuric minerals in rocks of the crust, as the ' original ' sulfur in volcanoes active or
inactive, as dissolved sulphate or dimethyl sulfide in seawater, and as ' trace gas ' the
atmosphere. In the human body though there was sulfur in the form of amino acids
such as methionine, cysteine and taurine, homosistein.
Sulfur Sulfur known by other names namely collection of solid yellow crystals
with the relative gravity of 2.07 at a temperature of 20 ° c. In the solid state, the
structure of the sulfur Rhombus-shaped and remains stable in this state until it
reaches a temperature oF 203 (95 ° c). Sulfur melts at a temperature of about 240 oF
(116 ° c) up to 300 oF (149 ° c). Warming up to 318 oF (159 oC) exceeds the rate of
polymerization of sulfur, will increase the value of viskositasnya. The above
temperatures oF 392 (200 ° c), the viscosity of sulfur will start dropping again. The
boiling point of the liquid sulphur around 824 oF (440 ° c) [2].
In the span between 121oC up to 143oC, used in the production of hot mix
asphalt and jobs (Hot Mix Asphalt, HMA), the viscosity of sulfur extended asphalt
(SEA) lower than hard asphalt. Sulfur has been used to modify the characteristics of
the Influence of Sulfur HMA against Marshall Asphaltic Conrete Wearing Course (AC-
WC) Arief Setiawan 25 base, binder and surface layer (Concrete & Course, 2010) [4].
Sulfur can be added into asphalt oil in hopes of giving change for a better mix
of characteristics and meet the specifications required by the Bina Marga in the
general specifications 2010 [3].
 Li/S batteries are one of the candidates suitable for the nextgeneration high
energy density batteries. However, the S cathode has several existing problems that
need to be solved. Some of the issues associated with the S cathodes include low
ionic/electronic conductivity of S and Li2S, large volume expansion of S (~80%
expansion) upon lithiation, and the dissolution of the intermediate products, namely
lithium polysulfides (Li2Sx, where 4 _ x _ 8), into the electrolyte. Various strategies
have been developed to solve these problems. While there has been extensive
discussions regarding the solutions for improving the ionic/electronic conductivity of
the cathodes and the volume expansion of S upon lithiation, the inhibition of
polysulfide dissolution into the electrolyte persists as the most important challenge.
Carbon nanotubes with fine pores have been successful in suppressing the
dissolution of polysulfides into the electrolyte. While, the use of glyme-based
electrolytes has been successful in suppressing the polysulfide dissolution [4].
Among these methods, one effective strategy to prevent LiPS from shuttling is
the modification of battery structure, for instance, building a physical barrier for LiPS
between the sulfur cathode and separator. Several kinds of carbon-based interlayer
have been applied to enhance the electrochemical performance the Li-S battery.
Although the interlayer provides an effective battery architecture, there is still a
drawback that the extra weight of the interlayer will reduce the overall energy density
[5].
We developed a sulphur dioxide plasma modification on a poly(methyl
methacrylate) (PMMA) material for fluidic electrophoresis devices. The inner surface
of the PMMA channel of a chip was modified by using sulphur dioxide plasma
treatment. Contact angle measurements indicated that the buffer solutions were able
to fill the capillary because of the hydrophilic property of the internal surface of the
chip. XPS analysis indicated that the sulphur dioxide plasma treatment introduced a
negative charge originating from the dissociation of the hydrogen atoms of sulphonic
groups. Since this introduced a negative charge originating from strong acid sulphonic
groups onto the surface of the channel, the electroosmotic flow (EOF) was observed
to be large (_7 · 10_4 m2 V_1 s_1) and stable over a wide range of pH (4–10). The
chip was fabricated by using plastic injection moulding methods for enabling the mass
fabrication and disposable use of chips. The separation method is based on the net
electric charge of the material, which enables the separation of identical samples on
the basis of both isoelectric points and molecular weight. Two synthetic peptides with
similar isoelectric points and molecular weights but different net charges were
selected as model protein samples for the separation. The sample peptides were
detected under fluorescence microscopy. The resulting electropherograms obtained
by using the sulphur dioxide plasma-treated PMMA chip demonstrated that the two
peptides were separated and that the migration time of the peptides was correlated
with the net charge [6].
The chemical warfare agent sulfur mustard (SM) can cause long-term health
effects that may occur even years after a single exposure. The underlying
pathophysiology is unknown, but epigenetic mechanisms are discussed as feasible
explanation. “Epigenetics” depicts regulation of gene function without affecting the
DNA sequence itself. DNA-methylation and covalent histone modifications
(methylation or acetylation) are regarded as important processes. In the present in
vitro study using early endothelial cells (EEC), we analyzed SM-induced DNA
methylation over time and compared results to an in vivo skin sample that was
obtained approx [7].
Sulfur ion (S6+) was incorporated into the TiO2 lattice using sulfur powder as
precursor.0.05% of silver was deposite dont he surface of Ti0.85S0.15O2 by photo
induced deposition method. The photocatalytic reactivity of TiO2, Ag–TiO2,
Ti0.85S0.15O2 and Ag–Ti0.85S0.15O2 photocatalysts were probed for the
degradation of a model compound congored (CR) dyeunder UV/solar light
illumination. FTIR and XPS results suggested that the dopant sulfurion (S6þ) was
incorporated into the TiO2 crystal latticeat Ti4þ lattice site and the sulfur ions on the
surface were modified as SO42− active sites serving as electron with drawing group [8].
The other is the poor conductivity of elemental sulfur and its final discharge
products (Li2S and Li2S2), causing extremely slow electrochemical kinetics for sulfur
redox process and low sulfur utilization. Rational design of sulfur cathodes are
urgently desired to solve these problems, and an effective strategy is to design
suitable carbon hosts to accommodate sulfur guest. Generally the carbon hosts
should meet two criteria. One is the selected carbon hosts need to possess high
conductivity, which can effectively improve sluggish electrochemical kinetic of pure
sulfur cathode and sulfur utilization. The other is the carbon hosts can alleviate the
“shuttle effect” during discharge/charge process [9].
In coal gasification, solid coal is converted to sulfur-free gaseous fuels for use
in electricity generation, as well as valuable chemical feedstocks. Reaction of
pulverized coal with limited oxygen and water at 800-1500oC produces a gas stream
consisting mainly of a 2/1 mixture of CO and H2. Under these conditions, sulfur in the
coal is reduced to H2S, which is removed through an acid-base reaction with a
nitrogen-containing compound such as ethanolamine (HOCH2CH2NH2). The resulting
salt is heated to release H2S, which is converted to elemental sulfur, a valuable
byproduct, by the Claus process [10].
Acid rain, a second major environmental problem, results primarily from the
production of sulfur dioxide, SO2, that accompanies the burning of sulfurcontaining
coal in power-generating plants. Sulfur dioxide is slowly converted to SO3 by reaction
with oxygen in air, and SO3 dissolves in rainwater to yield dilute sulfuric acid [11].
The primary cause of acid rain is industrial and automotive pollution. Each year
in industrialized countries, large power plants and smelters that burn sulfurcontaining
fossil fuels pour millions of tons of sulfur dioxide (SO2) gas into the atmosphere, where
some is oxidized by air to produce sulfur trioxide (SO3). Sulfur oxides then dissolve in
rain to form dilute sulfurous acid and sulfuric acid :
SO2(g) + H2O(l)  H2SO3(aq)
SO3(g) + H2O(l)  H2SO4(aq)
 Sulfur, can be extracted from petroleum products by a chemical process. Sulfur
is also mined by forcing hot water into underground deposits and pumping the liquid
sulfur to the surface. Percent yield is important in the cost effectiveness of many
industrial manufacturing processes. For example, the sulfur shown in Figure 11.9 is
used to make sulfuric acid ( H 2 S O 4 ) [12].

Another molecule that has resonance structures is sulfur dioxide, SO2, shown
in Figure 13. Sulfur dioxide released into the atmosphere is partly responsible for acid
precipitation.The actual structure of SO2 is an average, or a resonance hybrid, of the
two structures. Although you draw the structures as if the bonds change places again
and again, the bonds do not in fact move back and forth. The actual bonding is a
mixture of the two extremes represented by each of the Lewis structures [13]

Although sulfur is not a very abundant element (it constitutes only about 0.06
percent of Earth’s crust by mass), it is readily available because it occurs commonly in
nature in the elemental form. The largest known reserves of sulfur are found in
sedimentary deposits. In addition, sulfur occurs widely in gypsum (CaSO4 ? 2H2O)
and various sulfi de minerals such as pyrite (FeS2) (Figure 21.14). Sulfur is also
present in natural gas as H2S, SO2, and other sulfur-containing compounds. Sulfur is
extracted from underground deposits by the Frasch† process, shown in Figure 21.15.
In this process, superheated water (liquid water heated to about 160°C under high
pressure to prevent it from boiling) is pumped down the outermost pipe to melt the
sulfur. Next, compressed air is forced down the innermost pipe. Liquid sulfur mixed
with air forms an emulsion that is less dense than water and therefore rises to the
surface as it is forced up the middle pipe. Sulfur produced in this manner, which
amounts to about 10 million tons per year, has a purity of about 99.5 percent [14].

Over 60% of Iranian natural gases are contaminated with hydrogen sulfide or
other sulfur compounds. Khangiran refinery which receives around 50 MMSCMD sour
gas with 3.35 mol% H2S as its GTU feed, produces around 45% of Iranian sulfur
production. Three of the four existing sulfur recovery units (SRU’s) are initially
 installed more than 3 decades ago. Such relatively old Claus units with no tail gas
clean up facility have usually sulfur recovery efficiencies as low as 90%, due to the
low H2S content of the acid gas stream entering SRU process. Eliminating impurities
and contaminants such as carbon dioxide form SRU feed stream via proper acid gas
enrichment (AGE) process can effectively elevate the Claus combustion chamber
temperature and consequently increase the overall sulfur recovery efficiency of the
entire SRU process, to achieve more cleaner (SO2 free) air and higher purity product
(with brighter color).

Three different enrichment schemes are compared together and the most
effective and optimal scheme was selected based on their overall sulfur recovery
efficiencies. Coupled use of Aspen HYSYS and Promax software was employed to
simulate the entire GTU +enrichment section and SRU processes. It is shown that the
third scheme can successfully enrich H2S in the acid gas stream from its original
value of 0.335 (mole fraction) to more than 0.70. The optimal values of recycled acid
gas split ratio, recycled lean amine split ratio and enrichment tower pressure for this
scheme are found to be around 0.8, 0.14 and 60 psia, respectively.

To further reduce the sulfur dioxide emission of the entire refining process, two
scenarios of acid gas or air preheats are investigated when either of them is used
simultaneously with the third enrichment scheme. The maximum overall sulfur
recovery efficiency and highest combustion chamber temperature is slightly higher for
acid gas preheats but air preheat is more favorable because it is more benign. To the
best of our knowledge, optimization of the entire GTU +enrichment section and SRU
processes has not been addressed previously [15].

D. Methodes
1. Tools and Material
1.1. Tool

No. Tool’s name Category Image Tool Function

 appliance
1. Beaker As a solution

2. Measuring cup To measure the volume

of solution
1

3. Test Tube To the reaction solution

4. Analytical balance To weigh materials

5. Test tube rack To placea test tube

6. Bunsen burner Used in healting

7. Watch glass As a container of

substances to be
1 weighed

8. Grail evaporation As a container in the

heating/evaporation
1
 9. Spatula To take the substance
to be weighed
1

10. Batang Pengaduk

11. Drop pipette To take the solution

small amounts
1

12. Test tube clamp Pinning tes tube upon

heating
1

1.2. Table of Material

No. Name of material Category The physical Chemical properties

properties
1. H2O General  Clear liquid  Oxygen and
 Boiling point hydrogen are
100 0C covalently
bound
 A polar solvent
2. H2SO4 Special  Moleculer  Mineral acid
weight: 98.08 (inorganic) are
g/mol very strong
 Sulfuric acidin  Soluble in water
in the form of a in all
clear liquid, proportions
colorless, and
odories
3. BaCl2 Special  The molar mass  Soluble in water
of 3,856 g/cm3 and alcohol
 White solid  The crystal
structure of
 orthogonal
4. Na2SO3 Special  White solid  Can form
 The molar mass hydrates
of 126043 g/mol  A salt of sulfur
5. C12H22O11  White  Reactive with
solid/clear sulfur acid
6. Cu Special  Readdish  A metal element
yellow and  Reacts with the
shiny non-metalic
elements to
form ionic
compounds
7. HCl Special  Coloriess liqiuid  Soluble in water
 Molar mass  corrosive
36.46 g/mol
8. S Special  yellow powder  having many
allotropes in
nature
9. Kalium Kromat Special  
2. Experimental Work Scheme

Start

- Menimbang sebanyak 0,5 gr serbuk

belerang
- Memasukkan dan Memanaskan
perlahan-lahan belerang dalam cawan
penguapan
- Membiarkan membeku sampai
terbentuk kristal

Terbentuk Kristal berwarna

kuning

Finish
 Start

- Menimbang sebanyak 0,5 gr serbuk

belerang
- Memasukkan dan Memanaskan
perlahan-lahan belerang dalam cawan
penguapan
- Membiarkan membeku sampai terbentuk
kristal

Belerang berubah warna dari

kuning menjadi merah bata

- Menuangkan belerang yang baru saja

mendidih kedalam gelas kimia yang
berisi air
- Mengamati Kristal yang terbentuk

Terbentuk butir-butir Kristal

berwarna kuning

Finish
 Finish

- Memasukkan sekeping tembaga dalam

tabung reaksi yang berisi 1 mL asam
sulfat
- Memanaskan diatas pembakar Bunsen
- Mengamati perubahan yang terjadi

CuSO4 + gas H2

- Meletakkan kertas saring yang telah dibasahi

larutan kalium kromat yang di asamkan pada
mulut tabung reaksi
- Mencatat pengamatan

Kertas saring berubah warna

dari kuning menjadi biru

Finish

Start

- Menimbang sebanyak 0,5 gram sukrosa

- Memasukkan kedalam tabung reaksi
- Menambahkan 23 tetes asam sulfat pekat
- Mengamati perubahan yang terjadi

Terjadi perubahan warna dari

kuning menjadi hitam

Finish
 Start

- Memasukkan 2 mL asam asetat kedalam

tabung reaksi
- Menambahkan 2 mL etanol dan 2 mL asam
sulfat pekat
- Memanaskan tabung reaksi dengan
pembakar bunsen
- Mencatat hasil pengamatan

Menghasilkan bau seperti

balon (senyawa ester) dan
mendidih

Finish

Start

- Melarutkan larutan Na2SO3 secukupnya

dalam 3 mL air
- Menambahkan 3 tetes BaCl2 dan 3 tetes HCl
- Mengamati perubahan yang terjadi

Larutan berwarna
putih

Finish
E. Results and Discussion
1. Result

No. Treatment Observation result

A. Modification sulfur
1. - Weighing 0,5 grams in a cup - Sulfur Yellow
of sulfur and heat of
evaporation
- Bunsen burner heats up to - Sulfur melt slowly and do not change
melt above color
- Silence until frozen - Sulfur freeze
- Observe the change - Crystals formed yellow
2. - Considering 0,5 g of sulfur - Sulfur is in test tubes and colored yellow
and put into a test tube
- Heats and rattled a little test - The solution is yellow
tube
- Observe the change - The solution changed color to red brick
3. - Just pour boiling sulfur into a - Sulfur is in a beaker
beaker containing cold water
- Viewing crystals formed - Formed grain yellow crystal
B. The nature of sulfuric acid - Copper and sulfuric acid are in test tubes
1. - Entering se keeping the
copper in a test tube
containing 1 mL of H2SO4 - Copper-colored brick and cloudy
- Copper above a Bunsen
burner heats
2. - Pultting a filter paper that has - Filter paper is blue
been given a test tube
K2CrO4
- Observe the color change on - Filter paper is blue
filter paper
3. - Entering 0,5 g of sucrose into - Sucrose and sulfuric acid are in test
a test tube and add 23 drops tubes
of H2SO4
- Observe and record what - Changes color from yellow black
happens
4. - Entering 2 mL of acetic acid, 2 - Acetic acid ethanol and sulfuric acid
mL of ethanol, 2 mL H2SO4 are in test tubes
into the reaction tube
- Observe and record what - Aqueous smell like balloons and
happens boiling
5. - Dissolving Na2SO3 in 3 mL - Na2SO3 soluble
water
 - Add 3 drops of BaCl2 - The solution is white

- Adding 3 tetes HCl - No change occurred

2. Disscusion
The experiment on modification of sulfur, conducted an experiment with doing
thermal reactions (with warming). At first treatment, sulfur was reacted by way of
heating it until it melts and is yellow. After that the sulphur silenced and observed
lines of crystals that are formed. In this experiment the sulphur is experiencing
changes in microscopic or macroscopic. Changes in microscopic look at the
change of form and color change from solid to liquid sulfur, then becomes solid
again with a different structure, i.e. forming crystals. In addition changes in
makrosokopik that can be seen is a change in the color of yellow sulfur egg.
If reviewed by microscopic approach, there is a change in the structural form of
sulfur on the first form of sulfur rombik (α) which is composed of molecules of S8.
The results of the evaporation of sulfur it will produce Crystalline octahedral. The
experiment rombik sulfur is sulfur powder when heated until it melts produces
fused form of α and β sulfur sulfur with temperature modification about 95, 6oC.
When the heating is stopped and silenced berlerang, in microscopic sulfur back in
its original structure, i.e. sulfur α (rombik) and formed the lines of crystals. Lines
formed at this exact same sulfur Crystals such as ice cubes, where the lines of
Crystals that form elongated and yellow. In General, the reaction that occurs in
this experiment are:

Sα Sβ
 The next treatment step is done pretty much the same, that heats the sulfur.
This warming experiment performed until boiling sulfur and observe the changes
that occur. Based on observations, changes the color of the sulfur from yellow to
red brick. The sulfur has been boiling and then poured into the water and the
sulfur formed elastic, but immediately freezes. In General on this experiment
happened changes the structure of sulf ur are microscopic.

Figure 2
The sulfur has been simmering at the treatment above then enter into the beaker
containing water by means of boiling sulfur poured into the glass. These observations
generate sulfur Crystals shaped Crystal grains is yellow which does not mix with
water. The goal of the sulphur in the masukkannnya in a State of boiling into the
beaker containing water that is so that the molecules of sulfur did not have time to
form Crystals. Sulfur crystals that formed during this treatment such as plastic that are
burned. The crystals formed are usually on call with sulfur or sulphur-shaped plastic,
spiral chains. Sulfur sulfur is plastic that is formed when liquid is µ S is poured into
cold water. Consists of molecules such as chains and has a rubber-like quality when it
was first formed. But it subsequently became corrupted and may easily turn into sulfur
rombik.

Figure 3
 The next treatment aims to observe and identify properties of sulfuric acid from
each observation. First treatment namely by reacting a copper with H2SO4
concentrations through a process of heating but not to boiling. Based on the results of
the observations made, the reaction is indicated by the presence of the color change
from red brick becomes murky. In this experiment concentrated sulfuric acid used is
strong pengoksida substance. Sulfuric acid reacts with most metals via single
displacement reactions that generate hydrogen gas and metal sulfate. Reactions with
Tin and copper require hot sulfuric acid and concentrated, and this reaction will
produce sulfur dioxide than hydrogen. This is because the concentrated sulfuric acid
have a role as an oxidizing agent. So when hot concentrated acid reacts with copper,
zinc and Tin would produce salt, water and sulfur dioxide. Reaction equation:

Cu(s) + 2H2SO4(aq)  CuSO4(aq) + SO2(g) + 2H2O(l)

Figure 4

The next treatment that is putting pieces of filter paper that has been
moistened with a solution of K2Cr2O4 that has been pickled in the mouths of test tubes
containing copper heated and H2SO4. From the experiments that have been done are
obtained discolorations on the filter paper is white initially and then changed to blue.
The resulting blue color is caused by the formation of chromium (III) ion. Reaction
equation:
Cr2O72- + SO2 + H+  2Cr3+ + SO42- + 5H2O
 Figure 5

Subsequently reacting sucrose with concentrated H2SO4 0.5 grams in test

tubes. In this experiment, the sucrose which dissolves gradually concentrated H2SO4
ditetesi and yellow but gradually faded to black like caramel. The reaction equation is
as follows:
C6H12O6 + H2SO4  6C + 6H2O + H2SO4

Figure 6
From the above it can be seen that the reaction H2SO4 outlines sucrose or separate
atoms of hydrogen and oxygen from sucrose. Concentrated sulfuric acid is a powerful
dehydrating substances. Dehydration is the discharge of water molecules of a material
drawn by an ingredient for example H2SO4. The presence of carbon produced from this
reaction can be viewed from the formation of the black color on the mix when added with
concentrated H2SO4.

Then the fourth treatment i.e. reacting acetic acid, sulfuric acid, alcohol and then done
warming up. Prior to warming, the walls of the tube was hot, this is due to the presence
of the reaction between sulfuric acid against acetic acid and alcohol. Then do the
heating that produces air bubbles. Rekasinya equations:

CH3COOH + C2H5OH + H2SO4  CH3COOC2H5 + H2O

Based on the above reaction equations can note that the reaction is the reaction of
esterification, where alcohol was reacted with a carboxylic acid with an acid catalyst
generates the ester and water molecules. In this case it can also be seen that the
H2SO4 acted as a catalyst in the process of esterification. However, this reaction does
not appear any aroma essences as it should be. The distinctive smell of ester often
covered or distracted by the smell of a carboxylic acid.

The last treatment i.e. dissolve Na2SO3 in water and add some few drops BaCl.
According to the literature, these observations will produce colored deposits puth. The
reaction is formed as follows:

Na2SO3 + BaCl2  BaSO3 + 2NaCl

F. Conclusions
1. On the basis of practical work that has been done can be disimpilkan that the
sulfur contained in more than one crystal. The shape of the resulting Crystals are
usually yellow in color and shape depending on the temperature. Modifications of
sulfur into sulfur and sulfur rombik monoclinic.
2. The properties of sulfuric acid:
 Sulfuric acid as oxidizing agents:
Cu(s) + 2H2SO4(aq)  CuSO4(aq) + SO2(g) + 2H2O(l)
 Sulfuric acid as a dryer:
Cr2O72- + SO2 + H+  2Cr3+ + SO42- + 5H2O

 Sulfuric acid as a substance of dehydration:

C6H12O6 + H2SO4  6C + 6H2O + H2SO4
 Sulfuric acid as a catalyst:
CH3COOH + C2H5OH + H2SO4  CH3COOC2H5 + H2O
 Sulfuric acid if mixed with salt of nitric acid will produce:
Na2SO3 + BaCl2  BaSO3 + 2NaCl
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