Experiment 3

DETERMINATION OF MAGNESIUM AND CALCIUM IN NATURAL

WATER SAMPLES (AN ENVIRONMENTAL OVERVIEW)

Randy FIK. Karris[s11204071] | CH204 | 8th August [2pm-5pm]-22nd August

PRE-LAB
1. Water hardness is a result of various dissolved calcium, magnesium, or iron salts in
the river. Rocks are the principal source of calcium and magnesium in water. The
majority of calcium in surface waters comes from streams that pass over calcium-
containing rocks and minerals like gypsum, dolomite, and limestone.
2. 2(C17H35COO) Na + Ca+ (C17H25COO)2Ca + 2Na+
Soap + Calcium ion scum + Na+ ions
3. The 'scum' is caused by the reaction between the soap molecules and the calcium
(Ca2+) and magnesium (Mg2+) ions, which results in the creation of a grey-white
insoluble calcium and magnesium complex.

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INTRODUCTION
The interactions of rainwater with rocks and soils as it travels downhill greatly influence
the chemical composition of natural waters. At the surface of the earth, calcite (CaCO3),
dolomite (MgCa (CO3)2), and gypsum (CaSO4.2H2O) are frequently found in rocks. In
water with a mild acidity, all are soluble. Rainwater's mild acidity is caused by dissolved
CO2, which mostly produces weak carbonic acid, as well as some industrial pollutants.
Metal carbonates are released when rainfall comes into contact with the sediments and
rocks that contain them. This explains why the most prevalent cations in river water are
calcium and magnesium ions.

Our daily diet must contain a certain amount of magnesium and calcium for proper and
healthy development. However, there are numerous health risks that put human life in
danger if the concentration of these metals rises as a result of natural or human activities.

Drinking water is the most typical way to get these metal ions into your system. In many
nations, the majority of the water used for domestic purposes comes from creeks or rivers
that contain these metal salts. Measurements are typically taken from the water sources
that supply the nearby municipality on a regular basis to ensure the highest level of safety.
Utilizing EDTA is one of the best volumetric titration techniques for determining calcium
and magnesium. The analysis of water samples, such as tap water, soil extracts, water from
rivers, lakes, and wells, etc., can be especially benefited from this.

AIM
The purpose of this experiment is to become familiar with the analytical chemistry
methods, such as dilution, titration, and others, and to present results by way of
comparison on degree of accuracy and precision.

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EXPERIMANTAL
Materials
These are the instruments that are required for this experiment. Water samples (Tagabe
water sample and Prima water sample), volumetric flask, conical flash, indicator, and
EDTA

1. Standardisation of EDTA:
A magnesium salt can be used to standardize the EDTA solution, which is
currently around 0.01 M. An ammonia-ammonium chloride buffer is used to
maintain pH at 10 because the Mg-EDTA complex is only stable in alkaline
solution. Eriochrome Black T is the indicator because its solutions are unstable,
and sodium chloride is used as a diluent.
Make a standard magnesium solution by dissolving 0.2–0.3 g of MgSO4.7H2O in
water (100 cm3) in a volumetric flask, accurately weighed using the method of
difference, top pan, and analytical balance. Pipette out 25.0 cm3 of the solution,
add 1 cm3 of the ammonia/ammonium chloride buffer solution, a small amount of
indicator, and titrate with EDTA until the endpoint, which is when the color
changes from wine red to pure blue.
To obtain concurrent or extremely close (0.05 cm3) titre values, repeat the
titration. Using the findings, determine the molarity of the EDTA.
In your analysis of the water samples collected from the various locations and
filtered using Millipore filtration, you will use the standardized EDTA.
2. Analysis of Tap water:
100.0 ml of tap water should be pipetted into a conical flask.
"Added half a spatula of eryochrome and 1 ml of the buffer solution of
ammonia/ ammonium chloride."
"Black T indicator and standard EDTA titrated."
"The concentration of the ions present determines the end point. The transition
from red to purple to blue was "the same as in the previous part."
From this titration, "the total concentration of calcium and magnesium ions
[Ca2+] and [Mg2+] was determined."
At least three times of titration were performed in order to obtain at least two
concurrent or extremely close (0.05 cm3) titre values. lOMoARcPSD|28900255
The Mg ion concentration can therefore be determined by subtracting from the
result in the above sentence since this titration only yields the calcium ion
concentration.
3. Analysis of Water Samples [ Prima and Tagabe water sample]
In a 150 ml beaker, pour about 100 ml of the water sample.
"Pipeted out 62.5 ml and made up to the required amount (four-fold dilution)"
by "using distilled water."

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Shaken the volumetric flask to create a consistent solution.
"Then pipetted 25.0 ml into a conical flask with a capacity of 250 ml."
"Added half a spatula of eryochrome and 1 ml of the buffer solution of ammonia
and ammonium chloride."
"Black T indicator and standard EDTA titrate."
"At least three times of the titration were performed to obtain at least two
concurrent Titre values."
From this titration, "the total concentration of calcium and magnesium ions
[Ca2+] and [Mg2+] was determined."
"Pipeted out 25.0 ml of the diluted sample" into a conical flask with a capacity of
250 ml.
"Added 3ml of 2M sodium hydroxide solution and approximately 0.1 g of murexide
indicator and titrated with EDTA until the color changes from pink to purple," the
experimenter wrote.
"At least three times of the titration were performed to obtain at least two
concurrent Titre values."
"By subtracting from the outcome, the Mg ion concentration was calculated."

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RESULT
Part (1)
Table 1: showing Standardisation of EDTA calculation:

v=12.83ml/1000=o.o1283 L Molarity= 0.0099mol/L

n=c × v
n=0.0099 × 0.01283
n=1.27017×10−04mol

Part (2)
Table 2 (i): showing analysis of tape water part (a)
End point= purple to blue

Trials Initial burette Finial burette Titre volume (ml)

reading(ml) reading (ml)
1 0.00 9.70 9.70
2 9.70 24.00 14.30
3 24.00 38.50 15.50
Average = 12.83
Table 2 (a): showing calculation of the total concentration of calcium and
magnesium ion.

Mgs04.7H2o+EDTA+2H20 Mgso4(EDTA)+9H2O

Mole ratio [ca+2]= 0.00254mol/L

2H20: EDTA
2 : 1
X : 0.000127 X 2
X=0.000254 mole

n of [mg^+2,ca^+2 = 0.000254mol
v=0.1L
c=n/v
= 0.000254/0.1L
[mg+2]=0.00254mol/L

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 Table 2 (ii): showing analysis of tape water part (b).

Trials Initial burette Finial burette Titre volume (ml)

reading (ml) reading (ml)
1 0.00 21.00 21.00
2 21.00 44.10 23.10
3 14.3 35.00 20.50
Average= 21.53

Table 2 (b) showing calculation of the total concentration of [ca]

V=21.53ml/1000
=0.002153L
n=0.000127mol
[ca]=n/v
=0.000127/0.002153
=0.0059mol/L
Part (3)

Table 3 (I) showing analysis of Tagabe water part (a)

Trial Initial burette Finial burette Titre volume (ml)

volume(ml) volume (ml)
1 0.00 5.00 5.00
2 5.00 9.70 4.70
3 9.70 15.00 5.30
Average = 5.00
Table 3 (a): showing calculation of the total concentration of [ca+] and [mg+] in sample of
Tagabe river.

V=5.00ml/1000 n of ca=0.000127
=0.005L c=n/v
n of mg= 0.000127 =0.000127/0.005
[mg]=n/v =0.0254mol/L
=0.00127/0.005
=0.0254 mol/L

Table 3(ii): showing analysis of Tagabe water part (b)

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 Trials Initial burette Finial burette Titre(ml)
volume(ml) volume(ml)
1 0.00 5.30 5.30
2 5.30 10.40 5.10
3 10.40 15.60 5.20
Average = 5.20
Table 3 (b): showing calculation of the total concentration of [ca+] and [mg+]

V=5.20ml/1000 [mg]= 0.0254 – 0.02443

=0.0052L = 0.001 mol/L
[ca]=n/v
= 0.000127/0.0052
=0.024423mol/L

Table 4 (i): showing analysis of prima water sample part(a).

Trial Initial burette Finial burette Titre (ml)

volume (ml) volume (ml)
1 0.00 2.20 2.20
2 2.20 4.60 2.40
3 4.60 7.60 3.00
Average = 2.53
Table 4 (a): showing calculation of [ca] and [mg]

V=2.53ml/1000 n of [ca]=0.000127mol
=0.00253L c=n/v
[mg]=n/v =0.000127/0.00253
=0.000127/0.00253 =0.050mol/L
= 0.050mol/L

Table 4(ii): showing analysis of Prima water sample part(b).

Trial Initial burette Finial burette Titre (ml)

volume(ml) volume(ml)
1 0.00 4.50 4.50
2 4.50 10.30 5.80
3 10.30 16.20 5.90
Average = 5.40
Table 4(b): showing calculation of total concentration of [ca] and [mg]

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V=5.40ml/1000 [mg]=0.050-0.02352
=0.0054L =0.02648mol/L
[ca+]=n/v
=0.000127/0.0054
=0.02352mol/L

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DISCUSSION

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 CONCLUSION
The amount of dissolved calcium and magnesium in the water is a straightforward
definition of water hardness. Calcium and magnesium are the main dissolved minerals in
hard water. You might have noticed a film of residue on your hands after using soap to
wash them, depending on how hard your water is. "Soap scum" is created in hard water
when soap reacts with the water's relatively high calcium content. More soap or detergent
is required to get things clean when using hard water, whether it's your hands, hair, or
laundry.

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 REFERENCE
 . Quality of rivers of the United States, 1975 water year; based on the National
Stream Quality Accounting Network (NASQAN); 1977; OFR; 78-200; Briggs, John
C.; Ficke, John F.”
 . Tables for reducing bicarbonate to compute sum of determined constituents and
for calculating hardness of a natural ground water; 1960; OFR; 60-42; Dutcher, L.
C.; Moyle, W. R., Jr.”
 Ch204 lab handout

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