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Ivani K.

Suteno Practikum Report

A. Title
Observing Redox Reaction in Nitrogen Compounds
B. Objective
Study of the redox reaction of nitric acid and salts of nitrates, nitrites and redox
reactions redox reactions of ammonia and ions of ammonia.
C. Literature Review

Nitrogen is a diatomic molecule that has a triple bond. The bond energy is quite high so it
is very stable and difficult to react. Therefore most enthalpies and free energy formation of
nitrogen compounds are positive. This nitrogen molecule is very light and nonpolar so the
van der waals force between molecules is very small. This gas enters and exits the human
body when breathing without changing. This gas is odorless and tasteless. Nitrogen is very
necessary and is used as the manufacture of important compounds such as ammonia and
urea. Because of its high stability, nitrogen is used for oxygen protective gases in chemical
plants, metal industries and in the manufacture of electronic components. Liquid nitrogen is
also used to quickly freeze food [1].
Redox (short for reduction / oxidation reaction) is a term that describes the change in
oxidation number (oxidation state) of atoms in a chemical reaction. This can be a simple
redox process such as the oxidation of carbon that produces carbon dioxide, or the reduction
of carbon by hydrogen produces methane (CH4), or it can be a complex process such as the
oxidation of sugar in the human body through a series of complicated electron transfers. The
term redox comes from two concepts, namely reduction and oxidation. It can be explained
easily, oxidation explains the release of electrons by a molecule, atom or ion. While reduction
explains the addition of electrons by a molecule, atom or ion [2].
Nitrogen forms compounds in all oxidation states, from -3 to +5. Ammonia, NH3 is an
important commercial compound of nitrogen. Ammonia is a colorless gas with irritating and
stinging characteristics. Ammonia is made commercially through the Harber process of N 2
and H2. Ammonia is easily liquefied and the liquid is used as nitrogen fertilizer. Ammonium
salts, such as sulfates and nitrates are also used as fertilizer [3].
Nitrogen has an electron configuration of 1s2 2s2 2p3. In the formation of compounds with
other atoms, N atoms can obtain or more can be said to be shared with three electrons to
achieve valence skin octets 1s2 2s2 2p6. The oxidation number N in the compounds ranges
from -3 to +5. Diatospheric nitrogen N2 (g) is the main component of air (78% by volume),
then with the exception of precipitates for dichili and peruic NaNO3 deposits, nitrogen
compounds are not present in sufficient quantities on earth. This means that the source of N2
(g) and the manufacture of nitrogen compounds is the atmosphere. One important use of N 2
(g) is to provide (inert) sheaths for atoms, electronics, and chemical industry processes.
Liquid N2 is used as a frozen ingredient in the food processing industry. Another important
use is in the production of various nitrogen compounds, mainly through the manufacture of
NH3 [4].
There are a number of stable species in which, formally nitrogen valence skin is not full.
The best examples are NO, NO2, and R2N-O nitroxides, all of which have unpaired and
paramagnet electrons. The three-three NR3 covalent nitrogen is bipyramid: the bond is best
considered to contain sp3 hybrid orbitals so that electrons become solitary in fourth position
[5].
Nitrogen in the form of compounds is one of the nutrients. The presence of these nitrogen
compounds is needed for the formation of protoplasm. Consumers of nitrogen compounds in

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seawater are benthic algae and phytoplankton [6]. Compounds that have the ability to oxidize
other compounds are said to be oxidative and are known as oxidizers or oxidizing agents.
The oxidizing agent releases electrons from other compounds, so that itself is reduced.
Because he "accepts" an electron, he is also called an electron receiver. Oxidizing agents
are usually compounds that have elements with high oxidation numbers (such as H2O2,
MnO4−, CrO3, Cr2O72−, OsO4) or highly electronegative compounds, so they can get one or
two more electrons by oxidizing a compounds (eg oxygen, fluorine, chlorine, and bromine)
[7].
Ammonium and nitrite compounds are another form of inorganic nitrogen in ponds.
Inorganic nitrogen consists of ammonia (NH3-), ammonium (NH4+), nitrite (NO2-), and nitrogen
(N2). Biologically, the process of remodeling the metabolic waste of the cultivation biota can
become nitrate (NO3), a form that is not harmful in the nitrification process. Nitrogen is a
compound that is usually located in the uppermost layer in the sediment. Increasing the
speed of degradation will be achieved if the sediment is in aerobic conditions [8].
Oxidation by metals is a key reaction in organic synthesis. Hexavalent chromium
compounds are important, very powerful oxidizing agents suitable for organic synthesis.
Their most common applications are oxidation of primary and secondary alcohols to produce
Aldehydes, ketones, or carboxylic acids, depending on the reagents and conditions. Various
selective chromium (VI) oxidizing agents, for example, pyridinium chlorochromate (PCC),
pyridinium dichromate (PDC) and imidazolium dichromate (IDC) have been developed; This
allows oxidation of various compounds [9].
The close relationship between NO and adenosine in liver protection ischemic
preconditioning has been proven. Inhibition did not eliminate the effects of preconditioning
despite administration of adenosine, whereas adenosine deaminase infusion plus
administration did not fail to negate the effects of bene fi signal preconditioning. These
results suggest that the mechanism that leads to preconditioning in the ischemic liver
involves the release of adenosine, which induces the formation of NO [10].
Nitrous oxide is produced from enzymatic processes, including nitrification, nitrifier
denitrification, and denitrification mediated by microbes and fungi. The factors that regulate
the activity of nitrogen-cycling microorganisms—pH, organic matter, oxygen availability, soil
water content, soil texture, and supply of inorganic nitrogen—are often assumed to be the
same factors that regulate N2O emissions. Thermodynamics and kinetics of abiotic nitrous
oxide production in artificial solutions [11].
Lignin, the second most abundant renewable natural resource next to cellulose, is a
biopolymer having a highly branched three-dimensional structure. It is composed of three
phenylpropane units, p-hydroxyphenyl, guaiacol, and SyriCyl, which cross together by a
series of characteristic linkages such as C–C and C–O–C bonds. Industrial lignin is obtained
from the spent liquor in the biofuel and pulping industry as a by-product [12].
Redox mediators can be reversibly oxidized and reduced, thereby conferring the
capacity to transfer electrons between reduction and oxidation reactions. Redox mediators
are very important during the electron transfer process of anaerobic microbial respiration.
They accelerate the reaction by lowering the activation energy. Resulting in the enhanced
microbial transformation of pollutants and nutrients in ecosystems [13].
In redox reactions, electrons are transferred from one substance to another. The
reaction between magnesium metal and hydrochloric acid is an example of a redox reaction:

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Mg (s) + 2HCl (aq) MgCl2(aq) + H2(g)

An effect organic nitrogen compounds on deep hydrodesulfurization catalyst (CoMo/Al2O3)


has been carried out using micro-flow reactor at 5 MPa hydrogen pressure 1,5 h-1 liquid
hours space velocity, and 330 to 380 ˚c temperature [14]. Nitrogen is often used as an inert
background atmosphere in studies of electrode solids and reaction kinetics, studies of solid-
state transport phenomena, and in applications such as solid oxide fuel cells (SOFC),
sensors and membranes. Thus, the chemical and electrochemical reactions of oxides
associated with or with nitrogen should not be and are generally not considered [15].

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D. Methode
In this experiment using a qualitative method, the method used to identify a compound in
a sample.
1. Tools and materials
- Tools
No Name of Tool PictureTool Function Category

1. Reaction Tube To react samples of I


HNO3, Cu, H2SO4, KI,
KMnO4, Cu (NO3)2,
NaNO3, KNO3.

2. Chemical Glass as a container for distilled I


water

3. Glass measure to measure the volume of I


a solution of HNO3, NH3,
NaOH, and H2SO4

4. Shelf Test tube As the reaction tube I

5. Glass tubes Containers weighing I


chemicals NaNO3

6 Balance to measure the weight of II


Analytical the substance NaNO3, Cu
(NO3)2

7. Drop Pipette To take H2SO4, KI, I


KMnO4, Cu (NO3)2, HNO3
in small amounts

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8. Spatula To Take Cu (NO3)2 I


during the weighing
process

9. Penangas
To heat HNO3, CU, II
H2SO4, KI, KMnO4, Cu
(NO3)2, solutionsNaNO3

10. Clamp the tube To clamp the test tube I

11. Litmus paper Used to measure the pH I


of the solution

12. Erlenmeyer As an NHcontainer3 when I


heated

13. Scissors Used to cut copper wire I


and pH indicator paper

14. Bunsen burners Used to heat ammonia I


solution,KNO3 solidand
solid Cu (NO3)2 .

15. Measuring Used to dilute I


Pumpkin concentrated HNO3
solution.

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16. Stirring rod Used to stir the solution I


which will be reacted

17. Three feet As a support for asbestos I


gauze

- Materials
No Ingredient Category Physical properties Chemical properties of
name

1. Pieces Of General - Yellow-reddish and shiny - Is the element of metal


Copper (Cu) - His solid - Non metallic elements react
- Melting point 1083ºC with forming Ionic
- Boiling point 2595 ºC compounds

2. Nitric acid Specific - Molar mass 63,012 g/mol - Soluble in water


(HNO3) - Clear colorless liquid - Corrosive substance, toxic
- Melting point -42 ºC - Strong oxidizing agents and
- Boiling point 83 ºC strong acids

3. Sodium Specific - Solid white - Soluble in water, ethanol,


Hydroxide - Molar mass 39,9 g/mol and methanol
(NaOH) - Melting point 318 ºC - Insoluble in diethyl ether and
- Boiling point 1390 ºC a non polar solvent
- Strong base

4. Sulfuric Acid Specific - Molar mass 98,08 g/mol - Soluble in water


(H2SO4) - Hygroscopic, oily liquid, - Soluble in ethyl alcohol
colorless, odorless - Highly corrosive
- Melting point 10 ºC
- Boiling point 337ºC

5. Potassium Specific - Mass type 4,99 g/mol - Soluble in ether


Iodide (KI) - Yellow liquid - A non-polar solvent
- Melting point 11,4 ºC
- Boiling point 84,4 ºC

6. Aquadest(H2O) General - No smell, no taste - The universal solvent


- Boiling point 100 ºC - neutral pH
- Melting point 0 ºC

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7. Potassium Specific - Molecular weight 197,12 - Soluble in methanol


Permanganate g/mol - Strong pengoksida
(KMnO4) - Boiling point 32,5 ºC substance
- Melting point 2,83 ºC - Flammable
- Blackish purple crystalline
forms

8. Sodium Nitrate Specific - White color - Soluble in hot water, cold


(NaNO3) - Solid - Soluble in methanol
- Molecular weight 84,99 - Slightly soluble in acetone
g/mol
- Boiling point 308 ºC

9. Ammonia (NH3) Specific - The sharp-smelling - Easily soluble in water


- Melting point -77,73 ºC - Easy melting
- Boiling point -33,34 ºC - Corrosive in nature on the
- Molar mass 17,0306 g/mol copper and Tin

10. pH paper Specific - Red and blue - Litmus is red in acid solution
are red and blue colored
bases in aqueous solution
- The blue litmus is red in acid
solution and base in aqueous
solution is blue

11. Potassium Specific - Typical smell - Dissolved in water


Nitrate (KNO3) - Boiling point 400 ºC - Dissolved in liquid ammonia
- Melting point 334 ºC - Late in the glycerol

12. Copper Nitrate Specific - Shaped crystal blue - Very soluble in ethanol, water
(CuNO3)2 - Boiling point 170 ºC and ammonia
- Melting point 256 ºC

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2. Working scheme
 Nitric acid reaction with copper

Start

- Insert copper pieces into the test


tube
- Add two drops of HNO3

The Gas NO2 in


the solution is
blue

- 2 mL concentrated HNO3 thins to


obtain a solution of 7 M
- insert into the test tube
- add three pieces of copper

Gas bubbles
form

Finish

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 Nitric acid heating

Start

- Heat the solid KNO3 and solid


Cu(NO3)2
- Enter into the test tube
- Heat it
- observe the changes that occur

No change occurred in the


KNO3, while at CU(NO3)2
changes from solid to
liquid

finish

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 Nitrate reduction in base solution

Start

- Put 2 mL of 2 M HNO3 into a


test tube.
- Add dilute NaOH solution
- Add enough copper
powder/chips to state
- heat in water in a beaker

Changing colors in the


indicator of the orange
turned into red

Finish

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 Nitric acid redox reaction

Start

- Put 10 mL of dilute H2SO4in a test tube


- Cool for 5 minutes in a drsicator or use ice cubes.
- Put the cold sulfuric acid into the test tube side 1
gram NaNO3
- Divide the solution into 3 parts and put in each test
tube.
- Heat the test tube containing a solution of nitric acid
without adding another solution.

Brown’s gas
is formed

- For a second test tube


- Containing a solution of nitric
acid, add a little KI then heat it.

Changing colors in the


indicator of the red color
to the pale red color

-For the third test tube


containing a solution nitric
acid, add enough KMnO4
solution then heat it.

Not change
occured

Finish

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 Ammonia redox reaction


Start

- Put 10 mL NH3 into the Erlenmeyer


flask
- Make a spiral coil and smoldering
Cu wire then hang it in the mouth of
the Erlenmeyer flask.
- Heat the Erlenmeyer flask and
watch for sparks like sparks on the
Cu wire and pay attention to changes
in the solution

Not change occured

Finish

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E. Results and Discussion


1. Observation Results
No Treatment Result Observation
A. Reaction of nitric acid with copper

1. Insert the copper chip into the test tube Are in the test tube
Copper pieces

2. Add a few drops of HNO3 dilute Form NO2 gas a brown

1. Dilute 2 ml of HNO3 concentratedto a 7 M Solution There is a HNO3 solution 7


M

2. Insert into the test tube and add 3 pieces Bubble is formed small and large
of copper, observe the bubbles that occur

B. Heating of nitric acid

1. Heating KNO3 solid contained inside in the No change occurs


test tube

2. Heating Ca (NO3)2 solids contained in the The solid turns into liquid
test tube

C. Reduction of nitrates in alkaline solutions

1. Insert 2 ml of HNO3 2 M in a test tube There is a HNO3 solution 2 Min a test


tube

2. Add 5 ml of dilute NaOH solution There is a bubble

3. Add 3 pieces into a test tube containing There are many bubbles
NaOH solution and HNO3 2 M

4. Heats up in the water in the beaker The bubbles decrease and disappear

D. Redox reactions of nitric acid

1. Insert 10 ml H2SO4 into the test tube There is a solution of H2SO4 in a tube

2. Cool for 5 minutes using ice water The reaction tube is in ice water

3. Insert cold sulfuric acid into the tube NaNO3 dissolved in H2SO4
reaction that contained 1 g NaNO3

4. SolutionDivide into 3 pieces and put into a There are 3 tube solution H2SO4 and
test tubedifferent H2SO4

5. Heat up the tube reaction 1 observes In the clear solution, does not change
changes

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6. Heating the test tube 2 with the addition of Yellow, acidic solution with pH 2
KI. Litmus paper is used to check the
formed gas. Observing changes

7. Heating the test tube 3 with the addition of The thick purple solution changes to
KMnO4. Observing changes light purple

E. Ammonia catalytic oxidation

1. Inserting 10 ml of NH3 into the erlenmeyer There is an ammonia solution on


flask erlenmeyer

2. Making a spiral copper coil is not  For copper does not burn spiral
smoldering and a smoldering spiral, does not change
hanging on the mouth of erlenmeyer,  For copper, it was smoldering,
observing changes that occur there was no sparkling but the
copper was smoldering and then
dead

2. Discussion
Nitrogen is an inert gas at room temperature but is converted into nitrogen
compounds by the process of biological fixation through synthesis into the industry.
Nitrogen is also present in salts such as sodium and potassium nitrate. The network
of all living organisms contains nitrogen compounds in the form of proteins. Nitrogen
has an electron configuration of 1s2 2s2 2p3. In the formation of compounds with other
atoms, N atoms can obtain or more can be said to be shared with three electrons to
achieve valence skin octets 1s2 2s2 2p6. The oxidation number N in the compounds
ranges from -3 to +5. The maximum oxidation number corresponds to the VA class
number.

a. The reaction of nitric and copper acids


The first treatment is to insert the copper chip into the test tube by adding 2 drops
of concentrated HNO3. In this treatment, there is a change that is the formation of
brown NO2 gas and the copper chip dissolves in concentrated HNO3, this is because
concentrated HNO3 is a strong oxidizer so that copper chips can dissolve on HNO3.
The reactions that occur are:

HNO3(l) + Cu (s) → NO2(g) + Cu2+ (aq) + 2OH-(aq)


+5 0 +4 +2

+2 (oxidation)

-1 (reduction)

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Figure 1. concentrated HNO3 reacted with copper pieces

The next experiment was 2 mL diluted concentrated HNO3 which was in a test
tube added with 3 copper. In this treatment there is a change that is the presence of
gas bubbles, copper chips dissolve and color changes from clear to light blue. The
reactions that occur are:

3Cu(s) + 8HNO3(aq) 3Cu(NO3)2(aq) + 2NO(g) + 4H2O(l)


0 -2 +2 0
(oxidation)

(reduction)

Figure 2. Copper chips reacted with dilute HNO3

b. Heating nitric acid

Potassium nitrate (KNO3) is a natural source of nitrogen minerals. This


compound is classified as a nitrate compound with the chemical formula KNO 3. in this
experiment, we heat potassium nitrate by inserting the salt into a test tube, then
heating it. Once heated, potassium nitrate melts, and gas is produced. This indicates
the occurrence of thermal decomposition, according to the reaction equation as
follows:

2KNO3 (s) → K2O + 2NO2 (g) + 1/2 O2 (g)

Furthermore, heating Cu (NO3)2 produces a greenish blue melt. This indicates


that the reaction produces NO2 gas. The reaction is as follows:

Cu(NO3)2 (s) → CuO + 2NO2 (g) + 1/2 O2 (g)

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Figure 3. Solid KNO3 of Cu(NO3)2 after heating

c. Reduction of nitrates in alkaline solutions

Nitric acid is a strong oxidizing agent. In this experiment, we observed the


reduction reaction of nitric acid in alkaline solutions. The first step taken is 2 mL of
HNO3 added with 5 mL of dilute NaOH to produce a clear solution and cause
bubbles. The reactions that occur are:

HNO3(aq) + NaOH(aq) → NaNO3(aq) + H2O(aq)

Then add sufficient copper chip powder to the mixture of HNO3 added with
dilute NaOH which causes bubbles to multiply. When heated, bubbles start to
diminish and disappear and no color changes occur. The reaction is as follows :

3HNO3-(aq) + 8Cu(s) + 5 NaOH(aq) + 18H2O(aq) → NH3(aq) + 8[Cu(OH)4]-


+5 0 -3 +4
reduction

oxidation

d. Redox reaction of nitric acid


Redox (short for reduction / oxidation reaction) is a term that describes the
change in oxidation number (oxidation state) of atoms in a chemical reaction. In
the experiment 10 mL of dilute H2SO4 which was inserted into the test tube was
cooled for 5 minutes using ice cubes in order to make the gas formed from the
decomposition of NaNO3 a little. When cooled there is no color change, then mixed
with 1 gram NaNO3 until dissolved, when added with NaNO3 there is still no color
change (clear solution) because the reaction produces nitrite. Reactions that occur:

H2SO4 (aq) + NaNO3 (s) → NaHSO4 (aq) + HNO2 (aq) + 1/2 O2 (g)

Then the solution was put into 3 different test tubes. In the test tube 1 containing
nitric acid was not added with another solution while in tube 2 nitric acid solution was
added with KI and tube 3 of nitric acid solution was added with the KMnO4 solution,
then heated.

Tube 1: HNO2 solution

The heated HNO2 solution produces NO gas and a clear solution. This reaction
returns to produce nitrate compounds. The reactions are as follows:

3 HNO2 (aq) → HNO3 + 2NO (g) + H2O (aq)

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The above reaction is a disproportionation reaction (originating from the same


species) where nitrogen is oxidized to HNO3 by increasing the oxidation number from
+3 to +5 and experiencing a reduction (in NO) by decreasing the oxidation number
from +3 to +2.

Tube 2: HNO2 + KI solution

The HNO2 solution added with KI produces a clear solution with a yellow bias. At the
time of heating this reaction should take place in an acidic atmosphere and produce
NO colorless gas using indicator paper, but in this experiment, there was a change in
the color of the indicator paper at acidic pH 2.

Tube 3: HNO2 + KMnO4 solution

The mixture between the HNO2 solution and KMnO4 solution produces a purple
solution. This reaction takes place in an acidic atmosphere. The equation of the
reaction is as follows:

5NO2– (aq) + 2MnO4– (aq) + 6H+ → 5NO3– + 2Mn2+ +3H2O

Figure 4. Test tube 1,2,3 when heated

e. Catalytic oxidation of ammonia

In this experiment 10 mL of ammonia (NH3) was put into an erlenmeyer flask.


Then make a coil of Cu wire that is heated to a smoldering spiral. Furthermore, Cu
wire was hung above (in the mouth) erlenmeyer flask. Heat the erlenmeyer flask and
pay attention to sparks like sparks on the Cu wire and pay attention to changes in
the solution, there is no spark in this experiment but the copper is burning and then
dies.

Figure 5. The heating process of NH3 solution

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F. Appendix
1. Conclusion
the nitrogen element can undergo a redox reaction by reaction including nitric acid
reactivity test, nitrate salt reactivity test, and nitric acid and salt reactivity test. In some
of these reactions N undergoes changes in oxidation numbers. Reduction results from
nitric acid are influenced by its concentration, concentrated nitric acid produces NO2
and dilute nitric acid produces NO. It can be interpreted that the more concentrated
nitric acid, the less active and the greater the chance of producing NO 2. The higher the
concentration, the more concentrated the nitrate, the greater the ability to oxidize
copper. Nitric acid is oxidizing with iodine (I-) and as reducing agents with ion
permanganate (MnO4-). Nitric acid can react with metals in alkaline conditions that can
be tested using indicator paper.

2. Suggestions
In order for the practitioner to pay more attention to each existing procedure and to
be more careful in seeing any changes that occur.

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G. Reference
Journal
[1] Susana,tjutjut. (2004). source of pollutants and ammonia-nitrogen content in sea
water. Journal of analysis of ammonia content. Nasional Journal. Vol 29 (3) :
25-33
[2] Herlambang, Arie., Marsidi, Ruliasih. (2003). Denitrification Process With Biofilter
System For Wastewater Treatment Containing Nitrate. International Journal.
Vol 4 (1).

[3] Yuni Puji Hastuti. (2011). Nitrification and denitrification in ponds. Journal of
Indonesian Aquaculture. Vol 10 (1) : 89-98.

[4] Rumpa Saha et al. (2013). Choice of a suitable hetero-aromatic nitrogen base as a
promoter for chromic acid oxidation of DL-mandelic acid in aqueous media at
room temperature. Homogeneous Catalysis Laboratory, Department of
Chemistry. Interbational Journal. Vol 39 : 631-634.

[5] H. H. Ajamieh1, S, et all. (2004). Effects of ozone oxidative preconditioning on nitric


oxide generation and cellular redox balance in a rat model of hepatic
ischaemia reperfusion. Liver Internasional. Vol 24 : 55–62.

[6] Amanda R, et all. (2015). Biogeochemistry. Springer International Publishing


Switzerland. 126 : 251–267.

[7] Dongjie Yang. (2015). Structure and Properties of Sodium Lignosulfonate with
Different Molecular Weight Used as Dye Dispersant. Journal of Dispersion
Science and Technology. 36 (4) : 532-539.

[8] Guo, peng. (2018). Environmental pollution. Effect of long-term fertilization on humic
redox mediators in multiple microbial redox reactions. International Journal .
Vol 234 (1).

[9] Rana, S. Mohan. (2018). Effect of organic nitrogen compounds on deep


hydrodesulfurization of middle distillate. Journal Fuel processing technology.
177 (1).

[10] Valov Ilia and Bjoern Luerssen.( 2010). Activation Of Molecular Nitrogen At The Ir /
YSM Interface. International Journal of Electrochemical.Vol : 13.

Books

[1] Syukri. (1999). Basic Chemistry I. Bandung: ITB.


[2] Svehla,G.Vogel. (1985). Macro and Semimicro Qualitative Inorganic Analysis. Jakarta:
PT. Kalman Media Library.
[3] Achmad, Hiskia. (2001). Chemical Elements and Radiochemistry. Bandung: PT. Citra
Aditya Bakti.
[4] Petrucci. Ralph H. (1987). Basic Chemistry Principles and Modern Applied (Volume
3). Jakarta: Erlangga Publisher.
[5] Wilkinson. (1976). Basic Inorganic Chemistry. Jakarta: UI-Press.

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