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C. Literature Review
a. Literature Review of Disinfectant Analysis Experiment
Disinfection is the last barrier of wastewater reclamation process to protect ecosystem
safety and human health. However, the chlorination process results in the formation of
mutagenic/carcinogenic disinfection by-products (DBPs) deriving from the reaction of the
chlorine with organic compounds in wastewater. The effects of operating conditions (chlorine
dose, contact time, reaction temperature and pH value) of chlorination on the formation of
trihalomethanes (THMs) and haloacetic acids (HAAs) in biologically treated wastewater
samples were investigated in this study. The results indicated that the total THMs (TTHM) and
total HAAs (THAA) increased exponentially with increasing chlorine dose, but there are
discrepancies between the formation rates of TTHM and THAA. The THAA reached a peak at
contact time of 2 h and thereafter decreased with extended time. The formation time of THMs
depends on the wastewater content of quick or slow formers. The yields of bromated HAAs (as
MBAA, BCAA, and BDCAA) would decrease markedly after the contact time over 2 h during
wastewater chlorination, and were favored in low pH values of 4 and high pH values of 9 under
certain contact time. In addition, the formation of MBAA, BCAA, BDCAA decreased gradually
as reaction temperature increased from4 to 300C in the chlorination of wastewater containing a
certain concentration of bromide. The effects of operating conditions on THMs and HAAs
formation during wastewater chlorination were completely different from those of surface water
disinfection.
(Sun et.al, 2008)
The chlorine demand of a water is the difference between the amount of chlorine applied
and the amount of free, combined, or total available chlorine remaining at the end of the contact
period. The chlorine demand is different with different waters and even with a given water will
vary with the amount of chlorine applied, the desired residual, time contact, pH and
temperature. The test should be conducted with chlorine or with hypochlorite, depending upon
the form that will be used in practice.
(Sawyer,C.,N., 2003)
Trihalomethanes (THMs) are produced during chlorination of water. Only four THM
compounds normally are found: chloroform (CHCl3), bromodichloromethane (CHBrCl2),
dibromochloromethane (CHBr2Cl), and bromoform (CHBr3). Additional chlorination by-
products can be formed (including haloacetic acids and halonitriles; for example, see 5710D)
during the relatively slow organic reactions that occur between free chlorine and naturally
occurring organic precursors such as humic and fulvic acids. The formation potentials of these
additional by-products also can be determined, but different quenching agents and different
analytical procedures may be needed. Predictive models for estimating/calculating THM
formation exist, but because eventual THM concentrations cannot be calculated precisely from
conventional analyses, methods to determine the potential for forming THMs are useful in
evaluating water treatment processes or water sources or for predicting THM concentrations in
a distribution system. To obtain reproducible and meaningful results, control such variables as
temperature, reaction time, chlorine dose and residual, and pH. THM formation is enhanced by
elevated temperatures and alkaline pH and by increasing concentrations of free chlorine
residuals, although THM formation tends to level off at free chlorine residuals of 3 mg/L and
above; a longer reaction time generally increases THM formation.
Caporit
1 spatula of KI crystals
Amylum Indicator
Result
E. Observation Table
a. Observation Table of Disinfectant Analysis Experiment
No Treatment Observation Picture
1 Pour 25 mL of tap water - Tap water sample :
sample into Erlenmeyer colorless, odorless, and
glass by using volumetric normal temperature.
cylinder and give label
name of sample.
Picture :
Pour 25 mL of tap water
into erlenmeyer glass and
labelled
2 Add 1 spatula of KI crystal - KI crystal : white fine
into sample. powder, odorless, normal
temperature.
- After adding KI crystal, no
physical change happen
Picture :
Add 1 spatula of KI crystal
into sample
4 Add 2.5 mL of glacial - Glacial acetic : strong
acetic into sample by using odor, colorless, normal
measurement pipette and temperature.
propipette. - After adding glacial
acetic, sample become
colorless, strong odor, and
normal temperature.
Picture :
Adding glacial acetic into
samples
5 Add 3 drops of amylum - Amylum Indicator : clear
indicator into each sample and colorless
by using droplet pipette - After adding Amylum
Indicator, samples become
colorless, odorless, and
normal temperature
Picture :
Adding Amylum Indicator
into sample
Picture :
After adding KI crystal,
samples become orange
Picture :
Adding Amylum Indicator
into samples
Picture :
After adding Amylum
Indicator, samples become
dark brown
6 Titrate samples with - Natrium Thiosulphate :
0.0125 N natrium odorless, colorless, normal
thiosulfate by using temperature
measurement pipette and After tirtration, samples
propipette until the color of become clear and
sample become colorless. colorless.
The volume of tirtrate are
Picture :
8.5 mL = 44 mL
Tirtrate sample with
8.8 mL = 46.5 mL Natrium Thiosulphate
9.0 mL = 41.9 mL
Picture :
After titration, samples
become colorless
F. Discussion
The experiments of Analysis Technique of Environmental Pollution about disinfection
process and breakpoint chlorination is held at September 13th 2017 on 07.30 a.m until 10.30
a.m. This experiments held inside “B3 Effluent Laboratory”, Environmental Engineering
Department, FTSLK ITS. From all of the result of these experiments, we will get the residual
chlor from the first experiment and breakpoint of chlorination from second experiment by
calculating the doses of chlor and excess chlor of samples.
Tools that will be used on this experiment are erlenmeyer flask, measurements pipette,
propipette, volumetric cylinder, and spatula. Materials that will be used on this experiment is
water samples that taken from Hang Tuah River exactly at entrance gate (7°17'26.57"S
112°47'35.04"E) and tap water of water installation Environmental Engineering (7°16'46.60"S
112°47'33.72"E).
a. Discussion of Disinfectant Analysis Experiment
First experiment is about disinfectant analysis. Disinfection is the last barrier of
wastewater reclamation process to protect ecosystem safety and human health. However, the
chlorination process results in the formation of mutagenic/carcinogenic disinfection by-
products (DBPs) deriving from the reaction of the chlorine with organic compounds in
wastewater (Sun et.al, 2008).
The first step of this experiment is pour 25 mL of tap water sample into Erlenmeyer
glass by using volumetric cylinder and give label name of sample. Before we pour the water
sample into Erlenmeyer glass, we have to pour it first into 25 mL volumetric cylinder in order
to we can get appropriate volume. The characteristics of tap water sample are colorless,
odorless, and normal temperature. Practician have to give label in Erlenmeyer glass in order to
avoid mistakes of treatment of sample. Second step is add 1 spatula of KI crystal into sample.
The characteristics KI crystal are white fine powder, odorless, and normal temperature. After
adding KI crystal, no physical change happen in sample. The purpose of adding KI crystal is
to detect the presence of chlorine residue by react with KI. The reaction go through this
equation :
2ClO2 + 2I¯ → 2ClO2¯ + I2
Third step is add 2.5 mL of glacial acetic into sample by using measurement pipette and
propipette. The characteristics of glacial acetic are strong odor, colorless, and normal
temperature. After adding glacial acetic, samples become colorless, strong odor, and normal
temperature. The purpose of adding glacial acetic is to give acid condition in sample. The last
step is add 3 drops of amylum indicator into sample by using droplet pipette. The characteristics
of amylum indicator are clear and colorless. After adding amylum indicator, sample become
colorless, odorless, and normal temperature. The purpose of adding amylum indicator into
sample is as indicator of titration, so we can know the end point of titration. Actually, the next
step is titrate sample with 0.0125 N natrium tiosulfat until sample become colorless. But,
because after adding amylum, sample is still colorless, the titration process is not needed to do.
Because sample is colorless when added by amylum, we can conclude that tap water of
Environmental Engineering may does not contain residual chlorine because the chlorine already
evaporate in reservoir or it is already disappear in distribution process.
Forth step is add 2.5 mL of glacial acetic into each sample by using measurement pipette
and propipette. The characteristics glacial acetic are strong odor, colorless, and normal
temperature. After adding glacial acetic, samples become dark red, strong odor, and normal
temperature. The purpose of adding glacial acetic is to give acid condition in sample. The next
step is add 3 drops of amylum indicator into each sample by using droplet pipette. The
characteristics of amylum indicator are clear and colorless. After adding amylum indicator,
samples become dark brown, strong odor, and normal temperature. The purpose of adding
amylum indicator into sample is as indicator of titration, so we can know the end point of
titration. The last step is titrate samples with 0.0125 N natrium thiosulfate by using
measurement pipette and propipette until the color of sample become colorless. The
characteristics of natrium thiosulphate are odorless, colorless, and normal temperature. After
titration, samples become clear and colorless. The purpose of titration is to reduce iodine to
iodida through equation below :
I3- + 2S2O32- → 3I- + S4O62-
From data above, we can calculate doses of chlorine in each sample by using
following calculation :
Excess Doses of
Chlor Chlor
38.23 533.86
48.09 671.14
68.17 587.25
109.94 569.45
138.37 531.32
147.70 522
135.35 699.1
168.96 620.49
191.49 582.39
212.2 587.25
227.76 575.26
261.29 549.47
343.98 461.59
373.23 449.21
379.61 457
393.56 469.8
421.4 452.04
308.04 654.01
472.67 454.51
489.1 455.07
494.36 460.58
534.75 444.56
521.48 474.67
482.77 453.91
582.01 453.78
609.62 444.54
546.08 504.56
From table of excess chlor and doses of chlor, we can make comparison curve of doses
of chlorine and excess chlor.
600
Residual Chlor mg/L
500
400
300
200
100
0
452.04
533.86
671.14
587.25
569.45
531.32
699.1
620.49
582.39
587.25
575.26
549.47
461.59
449.21
469.8
654.01
454.51
455.07
460.58
444.56
474.67
453.91
453.78
444.54
504.56
522
457
From the graph above, we can know that the breakpoint chlorination is 654.01
mg/L. The amount of excess chlor in BPC is 308.04 mg/L and it does not fulfill the
standard of Indonesia Public Health Ministry Regulation 492/Menkes/per/IV/2010,
below 5 mg/L.
G. Conclusion
a. Conclusion of Disinfectant Analysis Experiment
After doing this experiment, we can conclude that the residual chlorine of tap water
of Environmental Engineering is 0 mg/L or it can be said does not contain residual
chlorine. So, tap water of Environmental Engineering is fulfill the standard of
Indonesia Public Health Ministry Regulation 492/Menkes/per/IV/2010, below 5
mg/L.
b. Conclusion of Breakpoint (BPC) Analysis
After doing this experiment, we can conclude that :
1. BPC of Hang Tuah water sample is 654.01 mg/L
2. The excess chlorine in BPC is 308.04 mg/L and it does not fulfill the standard
of Indonesia Public Health Ministry Regulation 492/Menkes/per/IV/2010,
below 5 mg/L.
H. Bibliography
a. Bibliography of Disinfectant Analysis Experiment
Sawyer, C.,N., Mc Carty,P.,R., Parkin,G.,F. 2003. “Chemistry for Environmental
Engineering and Sciences (5th ed)”. New York : Mc Graw Hill Companies.
Sun, Ying-Xue; Wu: Hu: Tian. 2008. “Effects of Operating Conditions on THMs
and HAAs Formation During Wastewater Chlorination”. Journal of Hazardous
Materials. Vol 168 : 1290.
b. Bibliography of Break Point Chlorination Analysis Experiment
American Public Health Association (APHA). 1999. “Standard methods for the
Examination of Water and Wastewater (20th ed)”. New York: American Public
Health, Association (APHA), American Water Works Association (AWWA),
and Water Pollution Control Federation (WPCF).
Kumar, Lokesh. 2013. “Study of double breakpoints during chlorination of river
Yamuna water, Delhi, India”. International Journal of Water Resources and
Environmental Engineering. Vol 5 (7) : 370.
Shovitri, Maya; Rosyidi; Nurhatika; Zulaika. 2011. “Apakah Breakpoint
Chlorination (BPC) Selalu Aplikatif Untuk Mengolah Limbah Cair Rumah
Sakit?”. Jurnal Purifikasi. Vol 12 : 84.
I. Question and Answer
a. Question and Answer of Disinfectant Analysis
Question :
1) Why determining chlor residue is important in drinking water installation?
2) Explain the important of contact time, chlor residue, and pH as a factor that effect
the strength of disinfection!
3) Calculate effective proportion of residue as HOCl and OCl- in pH = 6,8 and
temperature is 20oC!
4) Based on Chick Law, desinfection by chlorination follow first orde. How many
time thet needed to kill 99% bacteria with chlor residu 0,1 mg/L, if 80% dead
during 2 minutes in that dosage? (Kill = cxt)
Answer :
1) From chloride analysis we know minimum and maximum chloride total amount
used in water treatment so it can be used by consumer safely. Chloride is used in
get microbial bacteria that live in water pipe distribution over. Based on fullfill the
residual chlorine standard of Indonesia Public Health Ministry Regulation
492/Menkes/per/IV/2010, below 5 mg/L. And chloride standart from health
minister of Republic Indonesia 250 mL. It means that it’s still good enough if there
are residual chlor contain in water because it’s function to remove microbacterial
life in period of distribution time but in sufficient quantities and not excessive.
2) Contact time : (the time that chlorine is allowed to react with any impurities in the
water) are the most important factors. Chlorine needs time to inactivate any
microorganisms that may be present in the water being treated for human
consumption. The more time chlorine is in contact with the microorganisms, the
more effective the process will be. The contact time is the time from when the
chlorine is first added until the time that the water is used or consumed. As the
chlorine concentration increases, the required water-chlorine contact time
ultimately decreases.
Chlor residue : prevent pathogen microorganism to infect water in distribution
process. will remain in the water as it travels through the distribution system. To
support and maintain the chlorine residual, a process called re-chlorination is
sometimes done within the distribution system. This is done to ensure proper
chlorine residual levels are maintained throughout the distribution system.
pH : The type of chloramines that are formed is dependent on the pH of the water
prior to the addition of chlorine. Between the pH levels 4.5 and 8.5, both
monochloramine and dichloramine are created in the water. At a pH of 4.5,
dichloramine is the dominant form, and below that trichloramine dominates. At a
pH above 8.5 monochloramine is the dominant form. Hypochlorous acid reacts with
ammonia at its most rapid rate at a pH level around 8.3.
3) HOCl H+ + OCl- HOCl in temperature 20oC = 2.7 x 10-8
pH = - log [H+] [H+][OCl−]
= 2.7 x 10−8
6.8 = - log [H+] [HOCl]
t2 = 2,475 minutes
Answer :
1) For determining amount of optimum activated chlor that can be given in drinking
water treatment system in optimum disinfection process
2) Dosage of chlor that needed = BPC + chlor residues in water distribution system
3) Because application of BPC data for determining disinfection capacity, amount of
disinfection that needed and all of the things that corelate with disinfection process
in SPAM. BPC has reached when all of the substances that can be oxidiated already
oxidize. Ammonia was gone as N2 and still present in activated chlor. So if
correlated with application in SPAM, water already clean and safe for be used when
reached surface.
4) a. The best disinfection occurs at lower pH.
b. In waters with pH between 6.5-8.5, the reaction is incomplete and both species
(HOCl and OCl – ) will be present.
c. Best disinfection pH 6 - 7 but corrosivity concerns below pH 7.5
d. If you have high alkalinity and high pH (> 8) consider longer chlorine contact
time due to reduced efficiency of the hypochlorite form.
e. Chlorine (hypochlorite) is a strong base. Therefore, in a low alkalinity system, be
wary of pH changes with chlorination.
5) a. Q= 100 L/s
Cl2 = 60%
Cl2 residue = 2 mg/L
Q each day = 100 L/s x 86400 = 8,64 x 106 L/day
100
Amount of caporit that needed = x (Cl dosage + Cl residue) x Q
Cl2
100
= x ( 2 + 0,5) x 8,64 x 106
60
= 49 x 41,86
= 2051.14 L = 2,0514 m3
Total Volume = 2,05114 + 0,04186 = 2,093 m3