Environmental Laboratory Report

Permanganate Value
Arranged by
Environmental Engineering Class 2017

Jababeka Education Park, Ki Hajar Dewantara Street, Kota Jababeka, West Cikarang, Bekasi
17550 – Indonesia
Phone (021) 8910 9762-6, Fax (021) 8910 9768
Email: enrollment@president.ac.id, http://www.president.ac.id

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 SULPHATE
A. Objective
- To find the concentration of Sulphate in waste water
B. Introduction

The SO4 2- ion is one of the major anions occurring in natural waters. It is of importance in public
water supplies because ot its cathartic effect upon humans when it is present n excessive amounts. For
this reason the U.S. EPA’s secondary standard for SO 4 2- is 250 mg/L in waters intended for human
consumption. Sulphate is important in both public and industrial water supplies because of the
tendency of waters containing appreciable amounts to form hard scales in boiler and heat exchangers.
Sulphate is of considerable concern because it is indirectly responsible for two serious problems often
associated with the handling and treatment of wastewaters. These are odor and sewer-corrosion
problems resulting from the reduction of sulfate to hydrogen sulfide under anaerobic conditions, as
shown in the following equations:

High SO4 2- concentration as well as low pH conditions can result in streams that are fed by drainage
from abandoned coal mines and other exploited mineral-bearing deposits. The sulfide minerals
present are oxidized through a combination of bacterial and chemical action to produce H2SO4,

Not only does the SO4 2- content increase in streams to which mine drainage discharges, but the
lowered pH and high iron content produce added harm to water quality. For these reasons, care is
exercised today to replace the cover or to seal mines to prevent the introduction of O 2 and water that
lead to that reaction.

Principle

The sulfate ion (SO42-) in acidic condition reacts with barium chloride (BaCl 2) to form a barium
sulphate crystal (BaSO4) which is all the same. The beam absorbed by the barium sulfate suspension
were measured by the spectrofotometer and the sulfate content was calculated by comparison of the
reading with the calibration curve.
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C. Method
1. Calibration

1.1 Tools and Materials

Tools Materials
Pipette SO4
Bulb BaCl
Volumetric flask Buffer A
Cuvette
Spatula
Spectrophotometer

1.2 Procedure

No Steps Pictures
.
1. Prepare a measuring flask that has been
labeled with solution standard 0, 5, 10, 15,
20, 25 ppm

2. Calculate V (0,1,2,3,4,5) by equation

V1N1=V2N2 for each 25 ml solution
standard

Added V0 (0), V1 (1,25 ml) ,V2 (2,5ml)

,V3 (3,75 ml) ,V4 (5ml), V5 (6,25 ml) of
SO4

3. Added aquadest until 25 ml

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4. Add liquid buffer A 5 ml in each
measuring flask, make it homogenous

5. Add BaCl in each sample as much as one

spoonful of spatula, make it homogenous,

6. After that pour into the cuvette, but

beforehand rinsing it first with the cuvette
liquid itself

7. Clean cuvvete by tissue and than Insert the

cuvette into the spectrophotometer and set
it in advance

8. After that, count per 30 seconds in 4

minutes per solution standard to get max
wavelength and absorbance .

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9. Use the highest ABS for each solution
standard and creat a curve , R must more
than 90% , and get the the formula for
analysis SO4

2. Sample Analysis

2.1 Tools and Materials

Tools Materials
Spectrophotometer Tap Water
Erlenmeyer River Water
Beaker Glass BaCl2
Pipette Aquadest
Pipette Bulb
Spatula
Gloves

2.2 Procedure

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1. Prepare the apparatus that we want to use.

2. Pipette 25 ml of tap water and river water

and put in the beaker glass. (for the tap
water we can directly put in the
Erlenmeyer because don’t need to fitred)

3. Filter the river water with regular filter

paper and put in the Erlenmeyer.

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D. Experimental Result
1. Calibration

N1 = 100 ppm
N2 =25 ppm
N1 N2
V1 (ml) (ppm) (ppm) V2 (ml)
0 25 100 0
5 25 100 1.25
10 25 100 2.5
15 25 100 3.75
20 25 100 5
25 25 100 6.25

Wavelength = 304.5 nm
sample : 1 2 3 4 5 6
volume (ml) : 0 5 10 15 20 25
highest
number of 0 0.053 0.127 0.236 0.252 0.309
absorbent :

0.35

0.3 f(x) = 0.01 x + 0

R² = 0.97
0.25

0.2

0.15 Linear ()
Linear ()
0.1

0.05

0
0 5 10 15 20 25 30

Because R is more than 90% which R2 = 0.9721 so that curve and the formula that
we get is valid , the formula for analysis SO4 that we use is y= 0.0129x + 0.002.

2. Sample Analysis

Wavelength = 304.5 nm

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 Sample Time Absorbance Concentration (x)
(y) y= 0.0129x + 0.002

River 0 1.385 107.209302

1 1.385 107.209302
2 1.366 105.736434
3 1.365 105.658915
4 1.365 105.658915
5 1.369 105.968992
6 1.366 105.736434
7 1.369 105.968992
8 1.365 105.658915
0 0.427 32.9457364
1 0.428 33.0232558
2 0.430 33.1782946
3 0.433 33.4108527
Tap Water 4 0.432 33.3333333
5 0.435 33.5658915
6 0.435 33.5658915
7 0.437 33.7209302
8 0.437 33.7209302

Tap Water River water

1.39
0.44 1.39
0.44 1.38
1.38
0.43
1.37 E. Discussions
0.43 1.37
1.36 In this experiment we make standard solution
0.42
1.3633.2 33.3 33.4 33.5 33.6 33.7 33.8
32.9 33 33.1
105.5 106 106.5 107 107.5 from several value of standard, our standard
volume 25ml. We dilute 25 ml from 100ppm.
In order to get the data we use spectrometer as
our tools to find data. Firstly, we use second sample which 5 ml as finding the wavelength
and continue for each sample should get 8 data with 30minutes differences. The difficulties
during use this tool is before put the cuvette into the tools, make sure its already swab by
tissue so that the tools can work clearly and put the cuvette properly. To get valid data of
calibration for sulphate analysis, this result should be R > 90%. Following the requirement,
we got R from our result more than 90%. It can be said that our experiment follows as
calibration of sulphate.
For the sample analysis we take a sample from tap water and river water. We do the
experiment with direction from our lecturer and laboratory module. In this experiment we
want to find the sulphate value by using spectrometry of the tap water and river water
sample, and the result show in the graph, that show from the amount of the concentration. In

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our experiment the challenges is in the requirement that we have to be quick after adding the
BaCl2.

F. Conclusion

To get valid data of calibration for sulphate analysis, this result should be R > 90%.
Following the requirement, we got R from our result more than 90%. It can be said that our
experiment follows as calibration of sulphate. Because R is more than 90% which R2 =
0.9721 so that curve and the formula that we get is valid , the formula for analysis SO 4 that
we use is y= 0.0129x + 0.002 . For the sample analysis for sulphate we were able to get a
clear result and we were able to find the concentration from the equation that is found from
the calibration. In conclusion this experiment is important for analyzing the quality of water
especially considering that sulphate has many negative impacts.

G. References

AMONIUM

A. INTRODUCTION

Ammonia is a compound of nitrogen and hydrogen with the formula NH 3.It is a

colorless gas with a characteristic pungent smell, which very common in toilets
sometime. It is used in industry and commerce, and also exists naturally in humans and in
the environment. Ammonia is essential for many biological processes and serves as a
precursor for amino acid and nucleotide synthesis. The principle of ammonia is an
intensely blue compound, indophenols is formed by the reaction of ammonia,
hypochlorite, and phenol catalyzed by sodium nitroprusside. The interferences of NH3
are complexing magnesium and calcium with citrate eliminates interference produced by
precipitation these ions at high pH. There is no interference from other trivalent forms of
nitrogen. Remove interfering turbidity by distilled or filtration. If hydrogen sulfide is
present, it is removed by acidifying samples to pH 33 with dilute HCL and aerating until
sulfide odor no longer can be detected.

B. METHODS
Tools and Materials

Tools Materials
Pipette Phenol
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Bulb Na (nitroprusside)
Volumetric flask Oxidizing solution
Cuvette Aquadest
Spatula NH310 ppm
Spectrophotometer - River water

Alumunium Wrap - Drinking water

C. PROCEDURE
The steps of procedure on calibration curve for ammonia analysis are shown below:

No Procedure Picture

1 Prepare the tools and materials.

Make 6 working solutions with classifications below

in volumetric flask.

0 ppm 1 ppm 2 ppm 3 ppm 4 ppm 5ppm

Aquades Aquades Aquades Aquades Aquades Aquades

25 ml 22.5 ml 20 ml 17.5 ml 15 ml 12.5 ml

2.

NH3+ NH3+ NH3+ NH3+ NH3+ NH3+

0 ml 2.5 ml 5 ml 7.5 ml 10 ml 12.5 ml

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 Add 1mL phenol solution to each volumetric flask
3.
with through mixing.

Pour 1 mL sodium nitroprusside solution to each

4.
volumetric flask with through mixing.

Pour 2.5 mL oxiding solution to each volumetric

5.
flask with through mixing

6. Cover samples with alumunium foil film.

Let color develop at room temperature (22-27oC) in

7.
subdued light for 1 hour.

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 Pour each solution to the spectrophotometer cuvvete
8.
and wipe the surface with tissue.

Put it into the spectrophotometer light absorbance

9.
section.

Measure maximum wavelength (λ) in

10.
spectrophotometer.

11. Measure absorbance with maximum wavelength for

each solution in spectrophotometer.

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 Make a calibration curve based on the ppm and
12.
absorbance value.

Sample Analysis

No Step Picture

1. Take 25 mL sample river water and drinking

water into erlenmeyer flask

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2. Add with throughout mixing after each addition of
1 mL phenol solution, 1 mL sodium nitroprusside
solution and 2.5 mL oxidizing solution

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3. Cover samples with alumunium wrap

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4. Let color develop at room temperature (22 - 27 0C)
in subdued light for at least 1 h

5. Measure absorbance

D. EXPERIMENTAL RESULTS

Calculation of work solution needed

 0 ppm
Work solution needed = 0 mL

 1 ppm
V 1 N 1=V 2 N 2
(25 mL)(1 ppm)=V 2 (10 ppm)
V 2=2.5 mL

 2 ppm
V 1 N 1=V 2 N 2
( 25 mL )( 2 ppm )=V 2 (10 ppm)V 2=5 mL

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 3 ppm
V 1 N 1=V 2 N 2
( 25 mL )( 3 ppm ) =V 2 (10 ppm)V 2=7.5 mL

 4 ppm
V 1 N 1=V 2 N 2
( 25 mL )( 4 ppm )=V 2(10 ppm)V 2=10 mL

 5 ppm
V 1 N 1=V 2 N 2
( 25 mL )( 5 ppm )=V 2(10 ppm)V 2=12.5 mL

Result of Spectophotometry

λ max=657.5 nm

Normality Blank 1 2 3 4 5
(ppm)
ABS -0.000 0.486 0.798 1.320 1.541 2.721
3

2.5
f(x) = 0.49 x − 0.58
R² = 0.94
2

1.5 ABS
Linear (ABS)

0.5

0
0 ppm 1 ppm 2 ppm 3 ppm 4 ppm 5 ppm

Figure 1 Calibration Curve of NH3

Result Analysis

Blanko=0
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 river water = 0.074
Drinking water = 0.043
y = 0.4945x – 0.5829

River water
Y=0.074
Y = 0.4945x – 0.5829
0.074=0.4945x-0.5829
0.4945x=0.074 + 0.5829
0.4945x=0.6569
X=0.6569/0.4945
X=1.328

Drinking water
Y = 0.043
Y = 0.4945x – 0.5829
0.043=0.4945x-0.5829
0.4945x = 0.043+ 0.5829
0.4945x = 0.6259
X=0.6259/0.4945
X=1.265

Result

Dringking Water River Water

Y 0.043 0.074
X 1.265 1.328

E. DISCUSSION
In this experiment, a calibration curve was created by plotting absorbance vs. concentration (ppm)
in Excel. The calibration curve was constructed by measuring the absorbance rate of ammonia in six
standards solutions. From the experiment, we found that there are various reading of absorbance of
the ammonia after being detected by spectrophotometer. The highest readings that have recorded was
2.721 this was due to high concentration of ammonia in that water sample (5ppm). The graph from
Figure 1 shows that the high concentration of the ammonia the higher the absorbance. In order to
quantify how much ammonia is in our extract we measure the absorbance at a particular wavelength.
In the example, our measurements were at a maximum wavelength of 657.5 nm to coincide with the
ammonia peak and if it was at a lower wavelength then it would minimize interference from the
N H 3 peak. Our samples had concentration of 0, 1, 2, 3, 4, and 5 ppm. We put each of these in the
spectrophotometer in order to determine their absorbance.

F. CONCLUSION
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In order to figure out the relationship between concentration and color development standard curved
needs to be constructed from a series of samples of known concentration. The range of the concentrations
should be from zero to the maximum concentration detectable by the method. Series of solutions with
different colors only depend on the amount of concentrations within the samples.

To get valid data of calibration for ammonia analysis, this result should be R > 90%.
Following the requirement, we got R from our result more than 90%. It can be said that our
experiment follows as calibration of ammonia. Because R is more than 90% which R2 = 0.942 so
that curve and the formula that we get is valid , the formula for analysis ammonia that we use is
y = 0,4945x - 0,5829 . For the sample analysis for ammonia we were able to get a clear result
and we were able to find the concentration from the equation that is found from the calibration.
In conclusion this experiment is important for analyzing the quality of water especially
considering that ammonia has many negative impacts.

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