REPORT OF EXPERIMENTAL CHEMISTRY

Course: Experimental Analytical Chemistry III

DETERMINATION OF POTASSIUM AND SODIUM

CONTENT IN SOIL

BY:
Name : AYU KARTIKA
IDN. : 4143332004
Deoartement : CHEMISTRY
Program : CESP 2014
Group : II (TWO)
Ipmlementation Date : April, 2nd 2018

FACULTY OF MATHEMATICS AND NATURAL SCIENCE

MEDAN STATE UNIVERSITY
MEDAN
I. TITLE OF EXPERIMENT : DETERMINATION OF POTASSIUM AND
SODIUM CONTENT IN SOIL.

II. OBJECTIVE OF EXPERIMENT :

1. Can make calibration curve correctly.
2. Can determine the potassium and sodium content in soil (Belawan soil) with flame
photometry.
3. Knowing the function of addition reagent in K and Na standard solution.

III. THEORITICAL REVIEW

Land is the most important factor in the growth of plants in a cropping system, the
growth of a species is influenced by several factors, one of which is the availability of
nutrients, both macro and micro nutrients. Macro nutrients are required in relatively large
amounts such as C, H, O, N, P, K, Na, Ca, Mg, and S, while micro nutrients are required in
relatively small amounts such as Mn, Cu, Fe, Mo, B, and Cl (Astuti, 2004).
Potassium is a chemical element with symbol K (from Neo-Latin kalium) and atomic
number 19. It was first isolated from potash, the ashes of plants, from which its name derives.
In the periodic table, potassium is one of the alkali metals. All of the alkali metals have a
single valence electron in the outer electron shell, which is easily removed to create an ion
with a positive charge – a cation, which combines with anions to form salts. Potassium in
nature occurs only in ionic salts. Naturally occurring potassium is composed of three
40 40
isotopes, of which K is radioactive. Traces of K are found in all potassium, and it is the
most common radioisotope in the human body (Woodford, 2002).
Potassium is a silvery-white metal with a putty or wax-like consistency that is so soft it
can easily but cut with a knife. It is a member of the alkali metals, the group that contains
such elements as lithium and sodium. Like them, it is extremely reactive, and so is never
found in the free state in nature. Almost all potassium chloride that is mined is used as plant
fertilizer. In fact, plant and trees themselves were and early source of potassium for human
use (Stwertka, 2002).
Sodium is an extremely reactive, bright, silvery metal, light enough to float on water
and soft enough to be cut with a knife. It is far too chemically active to be found as a pure
elements in nature. even its storage presents a problem. It reacts violently with water,
producing enough heat, as it sizzles and bubbles on top of the water, to melt it. It is usually
kept immersed in a liquid such as kerosene to prevent it from reacting with air or moisture.
Sodium is the sixth most abundant element inthe Earth’s crust, present at a concentration of
2.63 percent by mass (Stwertka, 2002).
A centrifuge is a piece of equipment that puts an object in rotation around a fixed axis
(spins it in a circle), applying a force perpendicular to the axis of spin (outward) that can be
very strong. The centrifuge works using the sedimentation principle, where the centrifugal
acceleration causes denser substances and particles to move outward in the radial direction.
At the same time, objects that are less dense are displaced and move to the center. In a
laboratory centrifuge that uses sample tubes, the radial acceleration causes denser particles to
settle to the bottom of the tube, while low-density substances rise to the top (Susan, 2004).
Centifuge technology offers a wide range of modelling possibilities, but care has to be
taken in how the results are analysed and transferred to the real world. Centrifuge modelling
data should therefore always be used in comparison with other analytical, numerical or site-
specific studies. In respect of the interpretation and the further analysis, a designed test setup
of a centrifuge model, which can never be a full representation of a field situation, should be
as simple as possible to focus on the main influencing parameters (Springman, 2002).
Flame photometry is a branch of atomic spectroscopy in which the species examined in
the spectrometer are in the form of atoms. The other two branches of atomic spectroscopy are
atomic absorption spectrophotometry and inductively coupled plasma-atomic emission
spectrometry (ICP-AES, a relatively new and very expensive technique not used in Standard
base experiments). In all cases the atoms under investigation are excited by light. Absorption
techniques measure the absorbance of light due to the electrons going to a higher energy level
(Chatwal, 1979).
Flame photometry is suitable for qualitative and quantitative determination of several
cations, especially for metals that are easily excited to higher energy levels at a relatively low
flame temperature (mainly Na, K, Rb, Cs, Ca, Ba, Cu).This technique uses a flame that
evaporates the solvent and also sublimates and atomizes the metal and then excites a valence
electron to an upper energy state. Light is emitted at characteristic wavelengths for each
metal as the electron returns to the ground state that makes qualitative determination possible
(Skoog, et al., 1992).
IV. TOOLS AND MATERIALS
a. TOOLS
No Name of Tools Picture Size Quantity
1. Volumetric flask 50 mL 5 pieces

2. Centrifuge Tube - 2 pieces

3. Centrifuge Electric - 1 set

4. Measure Glass 25 mL 1 piece

5. Funnel - 1 piece

6. Beaker Glass 100 mL 1 piece

7. Watch Glass - 1 piece

8. Flame Photometer - 1 set

9. Filter Paper - 1 piece

b. MATERIALS
No Name of Picture Chemical Concen- Color Form Quantity
Materials formula tration
1. Soil Sample - - Brown s 1.5
grams

2. Ammonium NH4OAc 1N Colorless aq Sufficien

Acetate tly

3. Potassium KCl 250 ppm Colorless aq 77 mL

Chloridem
4. Sodium NaCl 100 ppm Colorless aq 75 mL
Chloride

5. Aquadest H2O - Colorless aq Sufficien

tly
V. WORK PROCEDURE
1. Making of Soil Solution

Making of Soil Solution

 1,5 grams of sample entered into

centrifuge tube.
 Added 10mL NH4Oac 1N solution
and closed with rubber.
 Placed the centrifuge tube in the
wooden holder above the electric
shaker, and shake for 60 minutes.
 Placed the tube into a centrifuge,
rotated at speed of 2000 RPM for 10
minutes.
 The colorless solution enter to bottle
film without the soil.

Result :
Soil sample + NH4OAc, the solution become two layers.

After rotated in centrifuge, the soil sample solution is not

homogen and save in the bottle for next experiment.
2. Determination of Potassium Soil
2.1 Standard Solution Series of Potassium (K)

2 ppm 5 ppm 10 ppm 15 ppm 20 ppm 25 ppm

 Dilluted with NH4OAc 1N in

measure flask 50 mL
 K standard solution read with
flame photometry

Result :
Standard solution 250 ppm dissolve with NH4OAc become colorless solution
with some concentration.

The read result of flame photometry:

2 ppm = 2,3 5 ppm = 3,1 10 ppm = 3,4
15 ppm = 3,1 20 ppm = 7,8 25 ppm = 22,3

2.2 Filtrate Sample

 Filtrate Sample

 Read with flame photometry

Result :
The color of solution is turbid.

The result of experiment is 5,6

3. Determination of Sodium Soil

3.1 Standard Solution Series of Sodium (Na)

5 ppm 10 ppm 15 ppm 20 ppm 25 ppm

 Dilluted with NH4OAc 1N in

measure flask 50 mL
 Na standard solution read with
flame photometry

Result :
Standard solution 100 ppm dissolve with NH4OAc become colorless solution
with some concentration.

The read result of flame photometry:

5 ppm = 8,5 10 ppm = 8,8 15 ppm = 10,2
20 ppm = 10,4 25 ppm = 11,5
 3.1 Filtrate Sample

Filtrate Sample

 Read with flame photometry

Result :
The color of solution is turbid.

The result of experiment is 10,7

VI. RESULT OF EXPERIMENT/REACTIONS/CALCULATIONS/DISCUSSIONS

1. RESULT OF EXPERIMENT
Table of Result Experiment
a. Making of Potassium standar curve
No KCl in NH4OAc (ppm) Emission Color
1. 2 2,3 Colorless
2. 5 3,1 Colorless
3. 10 3,4 Colorless
4. 15 6,5 Colorless
5. 20 7,8 Colorless
6. 25 22,3 Colorless

b. Determining of sample solution (K soil)

No Sample Emission Color
1. Soil Sample (Belawan Soil) 5,6 Turbid

c. Making of Sodium standar curve

No NaCl in NH4OAc (ppm) Emission Color
1. 5 8,5 Colorless
2. 10 8,8 Colorless
3. 15 10,2 Colorless
4. 20 10,4 Colorless
5. 25 11,5 Colorless

d. Determining of sample solution (Na soil)

No Sample Emission Color
1. Soil Sample (Belawan Soil) 10,7 Turbid
2. REACTIONS
 Soil Sample
Soil(s) + NH4OAc(aq) → Turbid solution

 Standard Solution
KCl(aq) + CH3COONH4(aq) → NH4Cl(aq) + CH3COOK(aq)
NaCl(aq) + CH3COONH4(aq) → NH4Cl(aq) + CH3COONa(aq)

3. CALCULATIONS
a. Making of K standard calibration curve
1) 2 ppm 4) 15 ppm
V1  ppm1  V2  ppm2 V1  ppm1  V2  ppm2
V1  250 ppm  50mL  2 ppm V1  250 ppm  50mL  15 ppm
50mL  2 ppm 50mL  15 ppm
V1  V1 
250 ppm 250 ppm
V1  0,4mL V1  3mL

2) 5 ppm 5) 20 ppm
V1  ppm1  V2  ppm2 V1  ppm1  V2  ppm2
V1  250 ppm  50mL  5 ppm V1  250 ppm  50mL  20 ppm
50mL  5 ppm 50mL  20 ppm
V1  V1 
250 ppm 250 ppm
V1  1mL V1  4mL
3) 10 ppm 6) 25 ppm
V1  ppm1  V2  ppm2 V1  ppm1  V2  ppm2
V1  250 ppm  50mL  10 ppm V1  250 ppm  50mL  25 ppm
50mL  10 ppm 50mL  25 ppm
V1  V1 
250 ppm 250 ppm
V1  20mL V1  5mL

Equation of standard curve

 Standard Curve of K
25

20
y = 0,722x - 1,708
15 R² = 0,720
Emission

10 Emission
Linear (Emission)
5

0
0 10 20 30
-5
K Concentration (ppm)

Based on the graph of the relationship of the concentration (ppm) and emission

(E) we get the line equation, y = 0,722x - 1,708 and R2 = 0,720 so the K concentration

can be calculated as follows:

 Sample of Belawan Soil

y = 5,6

by substituting the emission value of the sample solution at variable y then,

y  ax  b
y  0,722x - 1,708
5,6  0,722x - 1,708
5,6  1,708  0,722x
7,308  0,722x
7,308
x
0,722
x  10,122 ppm

So, the potassium (K) content in the Belawan soil is 10,122 ppm.

 Flame Emission

E  k .C
E  1,38.10 16 erg .k 1 .10,122 ppm
E  13,968.10 16 erg .k 1 ppm

b. Making of Na standard calibration curve

1) 5 ppm 4) 20 ppm
V1  ppm1  V2  ppm2 V1  ppm1  V2  ppm2
V1  100 ppm  50mL  5 ppm V1  100 ppm  50mL  20 ppm
50mL  5 ppm 50mL  20 ppm
V1  V1 
100 ppm 100 ppm
V1  2,5mL V1  10mL

2) 10 ppm 5) 25 ppm
V1  ppm1  V2  ppm2 V1  ppm1  V2  ppm2
V1  100 ppm  50mL  10 ppm V1  100 ppm  50mL  25 ppm
50mL  10 ppm 50mL  25 ppm
V1  V1 
100 ppm 100 ppm
V1  5mL V1  12,5mL
3) 15 ppm
V1  ppm1  V2  ppm2
V1  100 ppm  50mL  15 ppm
50mL  15 ppm
V1 
100 ppm
V1  7,5mL

Equation of standard curve

Standard Curve of Na
14
12
y = 0,152x + 7,6
10
R² = 0,951
Emission

8
6 Emission
4 Linear (Emission)
2
0
0 10 20 30
Na Concentration (ppm)
 Based on the graph of the relationship of the concentration (ppm) and emission

(E) we get the line equation, y = 0,152x + 7,6 and R2 = 0,951 so the Na concentration

can be calculated as follows:

 Sample of Belawan Soil

y = 10,7

by substituting the emission value of the sample solution at variable y then,

y  ax  b
y  0,152x + 7,6
10,7  0,152x + 7,6
10,7  7,6  0,152x
3,1  0,152x
3,1
x
0,152
x  20,39 ppm

So, the sodium (Na) content in the Belawan soil is 20,39 ppm.

 Flame Emission

E  k .C
E  1,38.10 16 erg .k 1 .20,39 ppm
E  20,138.10 16 erg .k 1 ppm

4. DISCUSSIONS

This experiment aims to study the working principle of the flame photometer and
determine the concentration of the sample solution by using a flame photometer containing
potassium and sodium. The working principle of this experiment is that when an element is
passed through a flame, it absorbs radiation energy, a number of atoms in an excited state in
the ground state will absorb energy from a characteristic wavelength and will reach a higher
energy state. In this experiment using soil samples that first made into a solution by way of
centrifugation. This method is used to determine the level of a metal in a sample based on the
emission of monochromatic light at a certain wavelength in a fluorescent or flame state. The
standard solutions used in this experiment were potassium solution (250ppm) and sodium
(100ppm).
 In this flame photometer it can be seen that most of the elements will be excited in a
flame at a certain temperature and emit radiation emission for certain wavelengths. Excitation
occurs when an electron from a neutral atom exits its orbitals to a higher orbital. And when
atom excitation occurs, the molecule will return to its original orbital and will shine light at
certain wavelengths. From the experimental results can be seen that the greater the
concentration of potassium and sodium elements, the greater the emission of the resulting
light.
The first stage in this lab is to make the soil solution by adding the soil with NH4OAc
then shake for 60 minutes. After that insert the solution into the centrifuge tube and insert it
into the centrifuge and rotate it with 2000 RPM speed for 10 minutes. It is intended that the
suspended particles in a container will settle to the bottom of the container due to the force of
gravity. After the soil solution through the centrifuge process, strain the solution. Filtrate
results from filtering will be measured using a flame photometer.
The next step is dilution of potassium solution from 250ppm by adding with NH4OAc
to be different concentrations, that is 2ppm, 5ppm, 10pp, 15ppm, 20ppm, and 25ppm. The
addition of NH4OAc solution is as buffer solution to maintain the pH of the solution. This
potassium solution is used as a standard reading. Next do a reading on the standard solution
to determine its concentration. It can be observed that at the time of reading the measured
sample the color is orange (orange) which indicates there is potassium inside. The result of
standard solution reading with several concentrations was 2,3; 3,1; 3,4; 6,5; 7,8; and 22,3.
Next, dilute the sodium solution from 100ppm to several concentrations, ie 5ppm,
10ppm, 15ppm, 20ppm, and 25ppm by adding the NH4OAc solution up to the boundary
mark. Then, re-measurement using a flame photometer that produces consecutive emissions,
8,5; 8,8; 10,2; 10,4; and 11,5.
The final stage in this lab is to read the diluted soil solution. Filter first the soil solution
that has been stored in the bottle by using filter paper. Grab the filtrate inside the beaker glass
and do a flame photometry reading to determine K and Na. The result of reading with soil
solution is 5.6 (K) and 10.7 (Na).
From experiments conducted it is known that the higher the concentration of a solution
then emission value of the flame will also be higher. This is in accordance with the theory
that the concentration of the solution is directly proportional to the value of the emission.
This is because the more metal particles will be the more excited that will return to the
ground state so that the emitted rays will more read as emissions on the Flame photometer
tool.
 Based on practice, it can be seen that the levels of Na = 20,39ppm in the Belawan soil
greater than the levels of K = 10,122 in the Belawan soil.
Based on the research that conducted by Bashir and friend (2016) in Khizarabad,
Sargodha, Pakistan showed that the soil of the studied area has high concentration of Na
(98,496 mg/kg). The plants grown on this soil show maximum growth so there is no need of
being amended with sodium containing fertilizer. While in this research note that Na content
on Belawan soil equal to 20,39 which indicate that Na content in Belawan soil less than Na
content at Khizarabad, Sargodha, Pakistan. So, the plants grown on Belawan soil show not
maximum growth so there is need of being amended with sodium containing fertilizer.
Based on the research was conducted, obtained the content of Potassium in Belawan
soil is 10,122. Meanwhile, based on the research was conducted by Harsha and Jagadeesh
(2017) in Haveri district, Karnataka showed that the soils varied appreciably in their physico-
chemical properties depending on nature and amount of parent material. The available
potassium in black soil varied from 322,56 to 752,64 kg ha-1 in surface layer. The higher
value of available potassium indicated that these soils were added with sufficient quantities of
potash fertilizers. From the above explanation can be seen that the Na content in Belawan soil
is much less compared with Na content in Haveri district, Karnataka. This shows that the soil
in India contains more nutrients suitable for gardening.

VII. CONCLUSIONS

1. Based on result the experiment of calibration curve obtained the line equation, y =

0,722x - 1,708 and R2 = 0,720 for K soil and y = 0,152x + 7,6 and R2 = 0,951 for

Na soil.

2. Based on the result of emission measurement using flame photometer for Belawan

soil sample, obtained the K concentration is 10,122ppm and Na concentration is

20,39ppm.

3. The function of adding NH4OAc solution is as buffer solution to maintain the pH of

the solution.
VIII. REFERENCES

Astuti, Y. (2004). Kandungan unsur hara kalium pada tanah dan tanaman (Acacia mangium
willd) studi kasus di HTI PT. Musi Hutan Persada, Sumatera Selatan. Bogor: Institut
Pertanian Bogor.

Basih, H., et al. (2016). Transfer of Sodium From Soil To Forage. IJAS. Vol. 1(2): 11 – 19.

BR, H., amd Jagadeesh, BR. (2017). Dynamics of Potassium In Selected Black Soil Type of
Haveri District, Karnataka. Journal of Pharmacognosy and Phytochemistry. Vol. 6(6):
2101-2106.

Chatwal, G. R., & Anand, S. K. (1979). Instrumental methods of chemical analysis. Jepang:
Himalaya Pub.

Skoog, D. A., West, D. M., & Holler, F. J. (1992). Fundamentals of Analytical Chemistry.
US: Saunders College Pub. Fort Worth.

Springman, S. (2002). Constitutive and Centrifuge Modelling: Two Extremes. Netherlands:

A.A. Balkema, a member of Sweets & Zeitlinger.

Stwertka, A. (2002). A Guide To The Elements, Second Edition. New York: Oxford
University Press, Inc

Susan R., Mikkelsen, and Eduardo Cortón. (2004). Bioanalytical Chemistry. New York: John
Wiley & Sons.

Woodford, Chris., (2002), The Elements: Potassium, New York: Marshall Cavendish
Corporation Tarrytown.

Medan, April, 19th 2018

Lecture Practicant

(Dr. Sri Adelila Sari, S.Pd, M.Si) (Ayu Kartika)

NIP. 197104102006042003 IDN. 4143332004