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Experiments 2 Calcium, Total Hardness, and Alkalinity Analysis
Experiments 2 Calcium, Total Hardness, and Alkalinity Analysis
Currently, EDTA titrations are among the most commonly used techniques to quantify
water hardness. This method relies on precise volumetric measurements and a lot of human
intervention, which slows down the procedure and limits efficiency. For this experiment we
measured the calcium and magnesium concentrations by using a fast and efficient instrumental
technique to eliminate these concerns, flame atomic absorbance spectroscopy (AA).
(Campbell & Peterson, 2010)
The major impact that chlorides impart on the receiving waters is the permanent hardness.
They are also known to increase the rate of sedimentation and thereby decreasing the water
column depth. When such effluents are disposed on land, chlorides tend to initially percolate
some distance, but over a period of time, they cause surface salt formation, thereby causing
increased alkalinity of the soil, thereby resulting in loss of soil fertility. Chloride in surface and
groundwater from both natural and anthropogenic sources, such as run-off containing road de-
icing salts, the use of inorganic fertilizers, landfill leachates, septic tank effluents, animal feeds,
industrial effluents, irrigation drainage, and seawater intrusion in coastal areas (Department of
National Health and Welfare, Canada, 1978). Chloride in water may be considerably increased
by treatment processes in which chlorine or chloride is used.
(Sagar et al, 2011)
c. Literature Review of Alkalinity Analysis Experiment
Water alkalinity and hardness are functions of the geology of the area and the percolation
of rain and surface water along with the dissolved carbon dioxide of the atmosphere. Rain water
is naturally acidic, which tends to dissolve some minerals more easily. Surface and groundwater
sources in areas with limestone formation are especially likely to have high hardness and
alkalinity due to the dissolution of bicarbonates and carbonates. Groundwater is considered as
the most desirable source of supply for aquaculture because it has more consistent diurnal and
seasonal physico-chemical parameters than surface water, and much less likely to be
contaminated by pathogens and mostly saline in nature. In aquaculture systems, compounds
that affect pH are generated continuously. The most influential of these are carbon dioxide and
ammonia. When carbon dioxide is added, hydrogen ions are released, the pH drops and the
water becomes more acidic. Ammonia works in the opposite way. Ammonia (NH3) can
combine with hydrogen ion (H+) to form ammonium (NH4+). Ammonium is less toxic than
ammonia, so, if the water is acidic, more of the ammonia will convert into ammonium, which
is less dangerous to the fish and prawn. However, more hydrogen in the water inhibits carbon
dioxide from converting carbonate ions.
(Raju et.al, 2014)
The pH of water is an intensity factor, while the acidity and alkalinity of water are capacity
factors. More precisely, acidity and alkalinity are defined as a water’s capacity to neutralize
strong bases or acids, respectively. The term “acidic” for pH values below 7 does not imply that
the water has no alkalinity; likewise, the term “alkaline” for pH values above 7 does not imply
that the water has no acidity. Water with a pH value between 4.5 and 8.3 has both total acidity
and total alkalinity. Alkalinity is usually the result of bicarbonate (HCO−3 ) and carbonate
(CO2−3 ) from dissolution of limestone, calcium silicate, and feldspars. Bicarbonate does not
exist in measurable concentration below a pH level of 4.5, so total alkalinity is measured by
titrating a sample with standard acid (usually sulfuric acid) to the methyl orange endpoint (pH
= 4.5), and the results are also expressed in terms of equivalent calcium carbonate. Waters with
pH values less than 4.5 do not contain alkalinity, while waters with pH values greater than 8.3
do not contain acidity.
(Boyd et.al, 2011)
D. Work Scheme
a. Work Scheme of Calcium Analysis Experiment
25 mL water samples
25 mL water samples
e. 2 mL pH 10 Buffer Solutions
25 mL water samples
10 drops PP indicator
H2SO4 0.01 N
Titrate each sample with sulfat acid, until the
sample’s colour change become colorless. Count the
concentration.
Result
*: if pH of samples is above 8.3, the practician have to do this step. But,if the pH is lower
than 8.3, the practician can direct add methyl orange to samples.
E. Observation Table
a. Observation Table of Calcium Analysis Experiment
normal temperature.
Picture :
After titration, the
sample;s colour become
purple.
Picture :
The sample’s colour
become dark purple
Picture :
pH of Hang Tuah river
water sample (out)
Picture :
pH of Puri river water
sample (in)
Picture :
The samples become
orange
Picture :
The sample’s colour
change become red
F. Discussion
The experiments of Analysis Technique of Environmental Pollution about calcium, total
hardness, and alkalinity analysis is held at Friday, September 6th 2017 on 07.30 a.m until 09.30
a.m. This experiments held inside “B3 Effluent Laboratory”, Environmental Engineering
Department, FTSLK ITS. From all of the result of these experiments, we will make bargraph
that contain of carbonate hardness, non-carbonate hardness, and total hardness so we can count
it. Then, we compare the result with Permenkes No. 492/Menkes/Per/IV/2010 in order to know
the appropriateness of each sample for drinking water.
Tools that will be used on this experiment are erlenmeyer flask, measurements pipette,
pro pipette, volumetric cylinder, spatula, and pH meter. Materials that will be used on this
experiment is water samples that taken from Hang Tuah River exactly at exit gate (70170260S
1120470350E) and Puri Neighborhood River exactly at entrance gate (70170260S 1120470290E).
a. Discussion of Calcium Analysis Experiment
First experiment is about calcium analysis. Calcium is an essential element for humans,
and is also responsible for water hardness, a water quality parameter frequently tested in
industrial plants and municipal water treatment facilities. Calcium is biologically required for
numerous functions, such as building and maintaining the bones and teeth, blood clotting,
transmitting of the nerve impulses and regulating heart's rhythm (Filik et.al, 2011). The purpose
and principal of this experiment is to determine amount of calcium (Ca2+) in water sample by
using titration method, with EDTA as an titrate and murexid as an indicator of equilibrium
point.
The first step of this experiment are prepare all of the tools and materials that will be used
in this experiments. After that, pour 25 mL of each samples (Hang Tuah river water (out) and
Puri river water (in)) into volumetric cylinder, then pour it into different erlenmeyer flask so
the volume of each erlenmeyer flask is 25 mL. The characteristic of both of sample are greenish,
stingy smell, and in normal temperature. The use of two different samples was aimed to know
the difference of Ca2+ content in both samples. The next step is add 1 spatula of murexid powder
into each samples by using metal spatula and then shake it well until mix completely. The
characteristic of murexide powder are dark purple gray fine, powder in form, and normal
temperature. Purpose of adding murexid powder is as an indicator of the titration, it will shown
when the optimum point has reached. After adding murexide, both of sample become violet and
odorless. The next step is add 2.5 mL of pH 12 buffer solution into each erlenmeyer flask by
using measurement pipette and propipette. The characteristic of pH 12 buffer solution are stingy
smell, colourless, and in normal temperature. After adding it, all of the samples become turbid,
violet, odorless, and still in normal temperature. Purpose of adding pH 12 buffer solution is to
keep the pH of the samples is at 12, from intervention of H+ ions. The next step is titrate the
samples with EDTA solutions by using measurement pipette and propipette, until the colour of
samples change become purple. The characteristic of EDTA solution are clear and colourless,
After titration, the colour of the samples become dark blue. Volume of EDTA solution to titrate
Hang Tuah sample are 2 mL while Puri sample are 2.7 mL. Purpose of tirtration by EDTA is
to made bonding between hardness ions with EDTA and natrium salt. Hardness is caused by
polyvalent metallion cations, though the divalent cations, such as calcium and magnesium
cations are usually the predominant cause of hardness. For example, when hard water is heated,
Ca2+ ions react with bicarbonate (HCO3-) ions to form insoluble calcium carbonate (CaCO3)
(American Public Health Association, 1999).
The last step is calculate amount of calcium ions in samples by following this step:
1000
Calcium (mg/L) = x a x N x 50
volume sample
Whereas :
a = mL of titration EDTA
N = normality of EDTA
Based on the equation, we can calculate the amount of calcium that dissolved in water
samples.
Hang Tuah Sample Puri Sample
1000 1000
Ca (mg/L) = x 2 x 0.03571 x 50 Ca (mg/L) = x 2.7 x 0.03571 x 50
25 25
Whereas :
a = mL of titration EDTA
N = normality of EDTA
Based on the equation, we can calculate the amount of calcium that dissolver in water
samples.
Hang Tuah Sample
1000
Total hardness (mg/L) = x 3 x 0.03571 x 50
25
= 214.26 mg/L
Puri Sample
1000
Total hardness (mg/L) = x 3.2 x 0.03571 x 50
25
= 235.686 mg/L
Whereas :
a = mL of titration HCl
N = normality of HCl
Based on the equation, we can calculate the amount of calcium that dissolver in water
samples.
Hang Tuah Sample
1000
Alkalinity (mg/L) = x 12.8 x 0.01 x 50 = 256 mg/L
25
Puri Sample
1000
Alkalinity (mg/L) = x 13.2 x 0.01 x 50 = 264 mg/L
25
From all of these experiments, we can calculate the hardness of each samples (carbonate
hardness, non carbonate hardness, and total hardness) by drawing the bargraph of each sample.
HCO3-
4.2
CH NCH
TH
Puri Sample
Table of mol equivalent of cation and anion in Puri sample
Cation mg/L Ar/Val meq/L Anion mg/L Ar/Val meq/L
Ca2+ 192.834 40/2 192.834/20 HCO3- 264 61/1 264/61
= 20 = 9.64 = 61 = 4.33
Mg2+ 235.686- 24/2 42.852/12
192.834 = 12 = 3.571
= 42.852
9.64 13.211
Ca2+ Mg2+
HCO3-
4.33
CH NCH
TH
H. Bibliography
a. Bibliography of Calcium 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).
Filik, Hayati; Aksu, Duygu; Apak, Resat. 2011. “Rapid Determination of Calcium in Milk and
Water Samples by Reflectance Spectroscopy”. American Journal of Analytical Chemistry.
Vol 2 : 276.
b. Bibliography of Total Hardness Analysis Experiment
Campbell, Jarryd; Peterson, Dan. 2010. “Determination of Water Hardness From Common
Water Sources Using Flame Atomic Absorbance Spectrometry”. Concordia College Journal
of Analytical Chemistry. Vol 1 : 4-6.
Sagar, A; Shruti, S; Kore, S. 2011. “Chloride Removal from Wastewater by Biosorption with
the Plant Biomass”. Universal Journal of Environmental Research and Technology. Vol 1(4)
: 416-417.
c. Bibliography of Alkalinity Analysis Experiment
Boyd, Claude E; Tucker, Craig S; Viriyatum, Rawe. “Interpretation of pH, Acidity, and
Alkalinity in Aquaculture and Fisheries”. North American Journal of Aquaculture. Vol 73 :
403-405.
Raju, P.A.R.K; Reddy; Raghuram; Babu; Rambabu; Kumar. 2014. “Alkalinity and Hardness
Variation in Ground Waters of East Godavari District due to Aquaculture”. International
Journal of Fisheries and Aquatic Studies. Vol 1 (6):121.
M+
[Mg2+] = x 50
BE
10 x 50
[Mg2+] = x 50
12,155
M+
[Sr2+] = x 50
BE
2 x 50
[Sr2+] = x 50
43,81
[Sr2+] = 2,282
Total Hardness = 37,425 + 41,135 + 2,282 = 80,842 mg/L
Temporary Hardness = Alkalinity
Temporary Hardness = 50 mg/L
Fixed Hardness = Total Hardness – Temporary Hardness
Fixed Hardness = 80,842 – 50
Fixed Hardness = 30,842 mg/L
2. Explain about 1) Total Hardness 2) Fixed Hardness 3)Temporary Hardness
Answer :
The total water hardness is the sum of the molar concentrations of Ca2+ and Mg2+,
in mol/L or mmol/L units. Although water hardness usually measures only the total
concentrations of calcium and magnesium (the two most prevalent divalent metal
ions), iron, aluminium, and manganese can also be present at elevated levels in some
locations. The presence of iron characteristically confers a brownish (rust-like)
colour to the calcification, instead of white (the color of most of the other
compounds).
Permanent hardness is hardness (mineral content) that cannot be removed by boiling.
When this is the case, it is usually caused by the presence of calcium sulfate and/or
magnesium sulfates in the water, which do not precipitate out as the temperature
increases. Ions causing permanent hardness of water can be removed using a water
softener, or ion exchange column.
Total Permanent Hardness = Calcium Hardness + Magnesium Hardness. The calcium
and magnesium hardness is the concentration of calcium and magnesium ions
expressed as equivalent of calcium carbonate. Total permanent water hardness
expressed as equivalent of CaCO3 can be calculated with the following formula:
Total Permanent Hardness (CaCO3) = 2.5(Ca2+ )+ 4.1(Mg2+)
Temporary hardness is a type of water hardness caused by the presence of dissolved
bicarbonate minerals (calcium bicarbonate and magnesium bicarbonate). When
dissolved, these minerals yield calcium and magnesium cations (Ca2+, Mg2+) and
carbonate and bicarbonate anions (CO32−, HCO3−). The presence of the metal
cations makes the water hard. However, unlike the permanent hardness caused by
sulphate and chloride compounds, this "temporary" hardness can be reduced either
by boiling the water, or by the addition of lime (calcium hydroxide) through the
softening process of lime softening.[4] Boiling promotes the formation of carbonate
from the bicarbonate and precipitates calcium carbonate out of solution, leaving
water that is softer upon cooling.
3. Explain 3 application of water hardness record that used in environmental engineering
Answer :
To design water installation for industry or home use
To know how to treat effluent water
To know how to treat drinking water