DIPLOMA IN INDUSTRIAL CHEMISTRY (AS115)

CHM 312 LABORATORY REPORT

(MAJOR PROJECT)
EXPERIMENT TITLE: DETERMINATION OF
POTASSIUM IN FERTILIZER
NAME:
NURSYAHIRAH BINTI ABDUL RAHIM (2011825426)

GROUP:
ASD5Dg

LECTURERS NAME:
ENCIK ZAILUDDIN BIN ARIFFIN

DATE OF EXPERIMENT:
19th AUGUST 2013

DATE OF SUBMISSION:
30th SEPTEMBER 2013
ABSTRACT:

The element that is to be determined is potassium in fertilizer by using Atomic

Absorption Spectroscopy. The fertilizer is obtained from three different brands which are
Tani, TST and Serbaguna that act as fruit inducer for plantation. The standard calibration
curve is used to plot all concentrations of standard solution in order to get correlation
coefficient that is 0.9991. The correlation coefficient must get triple nine to shows the
accuracy of experiment. The standard solution was prepared for concentration of 1 ppm,3
ppm,5 ppm, 7 ppm and 9 ppm. After that, three samples were prepared by using dilution
factor method. The samples were diluted in 250 mL and 100 mL volumetric flask. There are
two sets of results that needed to be obtained to compare which result is the best. Three
trials were ran for every brands for one set. The average concentration obtained for Tani,
TST and Serbaguna for first set is 2.4106 ppm, 0.2800 ppm and 8.5859 ppm respectively.
For second set, the average concentration for three samples from difference brands is
2.4216 ppm, 0.2804 ppm and 8.5758 ppm. The amount of potassium that contains in the
fertilizer for brand Tani, TST and Serbaguna is 24.06%, 2.80% and 85.76% by weight
respectively for the first set. For second set, the amount of potassium in three different
brands is 24.13%, 2.80%, and 85.52%. Fertilizer from Serbaguna shows the larger amount
of potassium compared fertilizer from TST and Tani.

INTRODUCTION:

Atomic Absorption Spectroscopy (AAS) is an instrument used for qualitative and

quantitative to determine several elements in given sample. This instrument involves four
difference processes which are nebulization, atomization, aspiration and volatilization. The
solution will be aspirated and nebulized to convert a liquid into fine spray or mist called
aerosol. Volatilization occurs where a liquid is convert into gaseous state. Atomization is
process of converting liquid into gas phase atoms or elementary ions.The flame AAS used in
laboratory UiTM Arau, Perlis is oxygen-acetylene .

The most common source for atomic absorption measurements is the hollow
cathode lamp. The cathode is made of metal of interest. It means that the different lamp for
each element. If the sample analyzed is potassium, so the hollow cathode lamp that will use
is potassium also. Hollow cathode lamp is used to maximize probability of redeposition on
cathode and also restricts the light direction. The detector used is photomultiplier tube which
can detect the element that need to be determined.

However, this instrument can detect varies element that range from parts per billion
(ppb) to parts per million (ppm). The advantages of using AAS are speed, convenience,
unusually high selectivity and moderate costs. The disadvantages are its sensitivity varies
with element, must maximize burner position and can detect only one element in one time.

In this experiment, the element analyzed is potassium in fertilizer. The fertilizer used
act as fruit inducer which the brands comes from Serbaguna, TST and Tani . Potassium is a
trace element found in fertilizer which is 17% by weight based on Nitrogen-Phosphorus-
Potassium (NPK) rating. Agriculture is the sector which uses the most amount of fertilizer for
plants production. There are many uses of potassium for plantation which are regulation of
water and nutrients movement in plant cells, promotes flowering and fruiting of the plants,
stimulates of an early growth, increases protein production, and improves resistances to
diseases and insects.

OBJECTIVES:

1) To determine the amount of potassium contains in fertilizer by using the standard

calibration curve.
2) To compare the experimental results with the values listed on the manufacturers
label.

PROCEDURE:

A) Preparation of Standard Solutions

1. 10 ml of 1000 ppm stock solution was pipetted. It was then transferred into 100
ml volumetric flask and it was diluted with deionized water to the mark. This
solution was labeled as 100 ppm.
2. 0.5 mL from 100 ppm solution was measured and was transferred into 50 mL
volumetric flask. It was diluted to the mark.
3. This solution was labeled as 1 ppm.
4. By using the 100 ppm and 50 volumetric flask, a series of standard solutions
having the following concentrations were prepared which are 3 ppm, 5 ppm, 7
ppm, and 9 ppm.

B) Preparation of sample (Tani, TST, and Serbaguna)

1. The fertilizer was grinded by using pestle and mortar.
2. By using analytical balance, it was weighed approximately of 2.5 g.
3. Then, the sample was dissolved with 150 mL deionized water in 250 mL beaker.
4. The solution was placed on a hot plate and boiled for 30 minutes.
5. It was then allowed to be cool and stirred thoroughly.
6. The solution was transferred into 250 mL volumetric flask and diluted to the mark.
7. It was filtered by gravity. 25 mL from the filtered solution was pipet into a 100 mL
volumetric flask. The solution was diluted to the mark.
8. The sample solution prepared was run for three times in order to obtain precision
results.

RESULT AND CALCULATION:

1) Preparation of Stock solution:

M1V1 = M2V2

(1000ppm) V1 = (100ppm)(100mL)

V1 = (100ppm)(100mL)

(1000ppm)

V1 = 10 mL
2) Preparation of Standard solutions:

Standard 1 (1ppm),

M1V1 = M2V2

(100ppm) V1 = (1ppm)(50mL)

V1 = (1ppm)(50mL)

(100ppm)

V1 = 0.5 mL

3) Samples calculation (Tani):

Average concentration obtained:

= 2.4336 + 2.4033 + 2.3949

3
= 2.4106 mg
L
The amount of K in sample (%wt/wt):

=2.4106 mg X 0.25 L
L
= 0.60265 mg X 100
2.505 g

= 24.06 %

Brands First trial (mg/L) Second trial (mg/L)

Run Run Run Average Run Run Run Average
1 2 3 1 2 3
Tani 2.4336 2.4033 2.3949 2.4106 2.4224 2.4237 2.4186 2.4216
TST 0.2809 0.2802 0.2790 0.2800 0.2827 0.2808 0.2778 0.2804
Serbaguna 8.5903 8.5879 8.5794 8.5859 8.5887 8.5797 8.5589 8.5758
Table 1

Brands First trial Second trial

Mass (g) % weight/weight Mass (g) % weight/weight
Tani 2.505 24.06 2.509 24.13
TST 2.504 2.80 2.508 2.80
Serbaguna 2.503 85.76 2.507 85.52
Table 2
DISCUSSION:

This experiment was conducted to determine the actual amount of potassium in three
different brands of fertilizers and to compare the experimental results with the values listed
on the manufacturers label. In this experiment, we use fertilizer as a sample from brand of
Tani, TST and Serbaguna. After it was grounded, we weighed approximately about 2.5 g
and dissolved it with 150 mL deionized water . Then, the solution was boiled for 30 minutes
to dissolved the fertilizer completely. The solution of sample was diluted and filtered to
remove precipitate in the solution in order to obtain clear solution.

When boiling process occur, the colour of sample solution from brand Tani is brown-
grey, TST is light blue while Serbaguna is very light blue. Dilution process was done for
three times. This dilution method is called dilution factor. The dilution process give colourless
solution for three samples. In order to obtained the concentration of sample in the standard
range, 5.90 mL from dilution in 100 mL volumetric flask was measured and diluted in 250 mL
volumetric flask. Two set of trials for every brands were conducted to compare which result
is the best one and also to see whether the condition of sample is change. The samples are
run for three times for one set of trial to get the average reading as recorded in Table 1.

The standard solution was prepared for five different concentrations which are 1
ppm, 3 ppm, 5 ppm, 7 ppm and 9 ppm. This standard solution was run to obtained
correlation coefficient that is 0.9991 before run the samples. This result can be shown from
graph of standard calibration curve which the absorption is directly proportional to the
concentration.

The percentage by weight of potassium for every brands of fertilizer were calculated
and compare to manufacturers label. The amount of potassium calculated is shown in Table
2 which are more than 17% by weight when compared with manufacturers label. However,
fertilizer from brand Serbaguna has a higher amount of potassium than the two brands for
two sets.The values obtained were shows a greater differences from label because of some
error while carried this experiment. First, the three samples are not grinded very well and
same size. This gives difference rate of reaction as difference surface area. Maybe some of
potassium does not breaks down completely and gives different amount of potassium.
Second, the solution was measured by using measuring cylinder which gives inaccurate
value. Third error is there have a slight variations in the eyes level while taking measurement
in measuring cylinder and burette which means eyes is not perpendicular to meniscus in
these apparatus.

The result shows that the concentration of potassium and weight of sample are
precise among three runs of both sets. The percent by weight also gives similar values for
both sets. In order to get this precision values, some precautions are needed to be aware
and take note. All glasswares used such as burette, beaker, volumetric flask and so on must
be rinsed and calibrated first before using them. The burette was ensured that there is no
bubble in the tip that will affect the reading obtained. . For this experiment, do not use
distilled water to dilute the standard and the sample, but use deionized water for dilution.
Deionized water is used in this experiment because it does not contain any charge. So that,
there is no attraction between difference charge of ion and thus affect the result. The scale
of the analytical balance must be set correctly based on the experiment.
CONCLUSION:

The amount of potassium that contains in the fertilizer for brand Tani, TST and Serbaguna is
24.06%, 2.80% and 85.76% by weight respectively for the first set. For second set, the
amount of potassium in three different brands is 24.13%, 2.80%, and 85.52%. Fertilizer from
Serbaguna shows the larger amount of potassium compared fertilizer from TST and Tani.

REFERENCES:

1) Analytical Methods for Atomic Absorption Spectroscopy, 12th August 2013, retrieved
from,
http://www.lasalle.edu/~prushan/Intrumental%20Analysis_files/AA-
Perkin%20Elmer%20guide%20to%20all!.pdf

2) NPK rating, 12th August 2013, retrieved from,

http://en.wikipedia.org/wiki/NPK_rating

3) D.A. Skoog, D.M. West, F.J. Holler, S.R. Crouch, Fundamentals of Analytical
Chemistry(8th Edition), Chapter 28: Atomic Spectroscopy, page 839-863.