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I. Title of experiment : Determination of the water hardness


II. Day, date of experiment : Wednesday, 29 October 2014
III. Purpose of experiment : Determining the hardness in water sample
IV. Basic Theory :
When refer to a hard water solution, mean a solution containing appreciable
amounts of calcium (Ca+2) and magnesium (Mg+2) ions. This hard water may include
other components such as solids, oil, dissolved gas, or other negative and positive
ions, but it is mainly calcium and magnesium ions dissolved in the water that make it
hard, thus tending to deposit scales of calcium carbonate (CaCO3) and magnesium
carbonate (MgCO3). Hard water is formed when water passes through or over
limestone or chalk areas and calcium and magnesium ions dissolve into the water.
The hardness is made up of two parts: temporary (carbonate) and permanent (non
carbonate) hardness. When water is boiled, calcium carbonate scale can form, which
can deposit on things like kettle elements. The scale will not stick to kettles that have
a plastic polypropylene lining but will float on the surface. The permanent hardness
that comprises calcium and magnesium sulphate does not go on to form scale when
heated or boiled.
The sample we used is sample water from well from area near Lapindo,
Porong. Water is an excellent solvent and readily dissolves minerals it comes in
contact with. As water moves through soil and rock near it, and it dissolves very small
amounts of minerals and holds them in solution. Calcium and magnesium dissolved in
water are the two most common minerals that make water "hard." Hard water requires
more soap and synthetic detergents for home laundry and washing, and contributes to
scaling in boilers and industrial equipment. For example the reactions:
Ca2+ + 2CH3(CH2)16COO-(aq)  Ca(CH3(CH2)16COO)2(s)
Hardness is usually expressed in terms of the equivalent quantity of calcium
carbonate (CaCO3) in milligrams per litre or parts per million. May also see hardness
expressed as Degrees of hardness in Clark (English) degrees, French or German
degrees. Interconversion between the different measurements can be made by using
the appropriate conversion factors below.

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There are no standard levels as to what constitutes a hard or a soft water. Table
2 gives an indication of the equivalents of calcium and calcium carbonate and the
relative degree of hardness.

While for Magnesium, that the threshold value of water hardness ranges
between 60 mg/L and 150 mg/L to overcome the entartrages pipes and its ability to
react with soap. No health-based guideline value for water hardness is proposed
(WHO, 1996) . Several studies have shown that the mortality from cardiovascular
disease is higher where the magnesium concentration in drinking water is less than 7
mg / L
To determine the hardness of a water sample, technologists use the EDTA
(ethylenediaminetetraacetic acid) titration. EDTA disodium salt is a soluble salt that
reacts readily with all +2 ions, namely Ca+2, Mg+2, Fe+2 and Ba+2. The EDTA anion
reacts quickly with any +2 metal to form a soluble metal EDTA complex. EDTA is
called a chelating or sequestering agent since it will react with and tie up heavy metal
ions and render them harmless to humans and water systems.
All metal-EDTA salts are colourless and require an indicator to tell us when the
reaction is over. Various hardness indicators have been developed. They all tell the
operator when the titration is complete. Hardness indicators are large complex
organic dyes that react with EDTA to form coloured complexes. EDTA reacts
preferentially with highly mobile metal ions, but once they are all tied up, the EDTA

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will react with the slow moving, massive dye molecules to give an endpoint. As a
consequence, endpoints are challenging.
We will use Eriochrome Black T for the total hardness endpoint, which includes
the sum of calcium and magnesium ions. Murexide indicator gives us the calcium
endpoint.

Ca2+ after added by murexid powder as indicator, the color is pink, and the end
point after titration is Ca2+ complex has purple color. While for magnesium If in a
water sample contained magnesium ions are then added to the EBT indicator of
magnesium ions (II) would bind EBT indicator. (H3In) produces a red complex (Mg-
In), if the solution is titrated with EDTA, the magnesium complex Mg-In will be
disconnected and form Mg-EDTA complex is more stable than the complex Mg-In,
while In is in a free state is blue. Titration was stopped when a clear blue color was
formed.
Mg 2+ + HIn2- (blue) → MgIn- (red) + H +
MgIn- (red) + H2Y2- → HIn2- MgY2- + H +
Calcium ions (II) can also react with the EBT produces Ca-inclusive complex, but the
complex is less stable than the complex Mg-In. Instead of Ca-EDTA complex is more
stable than Mg-EDTA complex. This means that if the solution contained only
calcium ions (II), and then titrated with EDTA, the discoloration will occur well
before the end point is reached. To overcome this deficiency, the calcium is added to
the analysis a little magnesium will bind more stable indicator.

MATHEMATICAL RELATIONSHIPS:
Molarity of EDTA solution is 0.01 N
mL of 0.01 N EDTA = 1 mg of CaCO3
EDTA molarity x EDTA volume (L) = Ca+2 molarity x Ca+2 volume (L)

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V. Tools and Mterials


1. Tools
Tools Scale Quantity
Beaker glass 10 ml 1
Volumetric pippete 10 ml, 25 ml 1, 1
Pro pipet - 1
Burette 50 ml 1
Erlenmeyer flask 100 ml 6
Graduated cylinder 10 ml 1
Clamp - 1
Statif - 1
Drops pippette - 10
Volumetric flask 100 ml 1

2. Materials
Materials Quantity
Water sample 150 ml
EDTAsolution 0,01 M As needed
EBT indicator As needed
NaOH 0,1 N As needed
Aquades As needed
Buffer solution pH 10 As needed
Murexid powder As needed

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VI. Procedure
1. Hardness of Ca2+ in water sample

25 ml

water sample

- Put into erlenmeyer flask 100ml using


volumetric pippete
- Added 1-2 ml NaOH 0.1 N
- Added 1 pinch of murexid power

Pink solution

- Titrated with EDTA solution 0.01 N


while shaken until the color changes
from pink to purple
- Noted the ml of EDTA that’s used
- Repeated 3 times

Volume of
EDTA solution

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2. Hardness of Mg2+ in water sample

1 ml sample

- Diluted 100 times using volumetric


flask (The sample is diluted because the
EDTA that’s used is more than 15ml)

25 ml diluted sample

- Put into erlenmeyer flask 100ml using


volumetric pippete
- Added 1-2 ml buffer solution pH 10
- Added 1 drops of EBT indicator

Pink solution
- Titrated with EDTA solution 0.01 N while
shaken until the color changes from pink to blue
- Noted the ml of EDTA that’s used
- Repeated 3 times

Volume of
EDTA solution

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VII. Result of experiment

Procedure Before After Reaction / hyphotesis Conclusion

1. Hardness of Ca in water sample Color of solution 1. Sample + NaOH = colorless - 2Ca2+ + 2NaOH→ - The hardness of
*sample: colorless 2. After added by murexid Ca(OH)2 + 2Na+ Ca2+ in the
*NaOH: colorless powder the color changed to - Ca2+(aq)+EDTA4-(aq)→ sample is 9,6
*EDTA: colorless pink. Ca(EDTA)2-(aq) mg/l
3. After titrated by EDTA the - Threshold of Ca2+ - Because the
Murexid powder: color changed to purple. hardness is
black 4. The EDTA solution that is Ca2+ is less
used: than 30, the
V1= 1,2 ml hardness level is
V2= 0.5 ml low.
V3= 1,0 ml
-
5. The hardness of Ca2+ in the
water:
V1=19,2 mg/L
V2= 8 mg/L
V3= 1,0 mg/L
6. Average of the hardness of
Ca2+ in the water is: 9,6 mg/L

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Procedure Before After Reaction / hyphotesis Conclusion

2.The hardness of Mg in water sample Color of solution 1. Sample + NaOH = colorless - Mg2+(aq)+EDTA4-(aq)→ - The hardness of
*sample: colorless 2. After added by EBT indicator Mg(EDTA)2-(aq) Mg2+ in the
*Buffer pH 10: 1 drop the color changed to - the threshold value of sample is 1344
colorless pink (+++) water hardness in mg/l
*EDTA: colorless 3. After titrated by EDTA the magnesium ranges Because the
*EBT indicator: color changed to blue. between 60 mg/L and hardness is
purple 4. The EDTA solution that is 150 mg/L to overcome Mg2+ is more
used: the entartrages pipes and than 150mg/L,
V1= 1,5 ml its ability to react with the hardness
V2= 1.2 ml soap. For drinking water level is high.
V3= 1.5 ml is less than 7 mg / L
5. The hardness of Mg2+ in the -
water:
V1=1440 mg/L
V2= 1152 mg/L
V3= 1440 mg/L
Average of the hardness of Ca2+
in the water is: 1344 mg/L

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VIII. Analysis and discussion

The experiment was conducted aims to determine hardness in the water, where we
do some experiments to determine the calcium hardness and magnesium hardness
of well water samples. At this hardness lab, samples were taken from wells in the
area around the Lapindo mud, Porong.
Hardness of Ca2 + in water sample

Determination of hardness of + in water wells around the Lapindo mud, Porong,


that is by pipette with pipette goiter 25 ml sample is then inserted into a 100ml
Erlenmeyer flask and supplemented with 1 ml 0,1N NaOH solution, the addition
of NaOH was used to precipitate Ca2 + to Ca(OH)2. However, this does not lead to
the addition of NaOH sediment, possibly due to the solubility of Ca(OH)2 is quite
high and after the addition of NaOH to the solution remained colorless. The
reaction is as follows:

2Ca2+ + 2NaOH→ Ca(OH)2 + 2Na+

After that, add 1 pinch of murexid powder. The addition of this indicator serves
as a complexing agent that produce a specific color. The addition of the indicator
resulting pink solution. Furthermore titrated with 0.01 N EDTA solution while
continuing to be shaken, so that the end point of the titration can be observed with
a color change from pink to purple. Reaction as follows:

Ca2+(aq)+ EDTA4-(aq)→ Ca(EDTA)2-(aq)

After replications 3 times, then the volume of EDTA required for titration of Ca2 +
in the hardness titration 3 times, respectively for V1 = 1.2 ml; V2 = 0.5 ml; V3 =
1.0 ml, which is then used to calculate the hardness of Ca2+ by using the
following formula

A  C 1000  MrCa
Ca 2 (mg )   pengenceran
L Vol.sampel (ml )

and obtained hardness Ca2 + in V1 = 19.2 mg / L; V2 = 8 mg / L; V3 = 11.6 mg /


L, in order to obtain hardness Ca2 + average for the third titration is equal to 9.6

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mg / L. If seen in the table threshold of Ca2 + in water, hardness values of Ca2 +


that we get, including the low level of hardness.

Hardness Mg 2+ in water sample

In the determination of the hardness of Mg 2+, the sample treatment was the
same as the sample on the determination of the hardness of calcium (Ca), but for
the procedure is slightly different due to the determination of the hardness of Mg
2+
is need to be diluted 100 times, it was done because EDTA solution used for
titration is greater than 15ml. The first step taken is pipetted sample using a
volumetric pipette 1 ml, then inserted into a 100ml volumetric flask. Then added
with distilled water to the mark. Subsequent treatment of the pipetted sample has
been diluted as much as using a pipette 25ml. After that, the samples were added
with buffer solution pH 10 as 1ml. The addition of a buffer solution is aimed at
the creation of Mg(OH)2 to easily determine the Mg in solution. The addition of a
buffer solution resulted in a clear solution, then added a bit of EBT indicator until
the solution changes color to pink. The function of the addition of EBT indicator
is as complexing produce a specific color. Furthermore, EDTA is titrated with
0.01 N while stirring, stirring until it changes color. EDTA is added as a titrant,
magnesium will be a complex, and when all the magnesium has become a
complex solution changes from pink to be the color blue signifies the end point of
the titration. The reaction is as follows:

Mg2+(aq)+ EDTA4-(aq)→ Mg(EDTA)2-(aq)

After replications 3 times, then the volume of EDTA required for titration of
Mg2+ hardness titration 3 times in a row by V1 = 1,5ml; V2 = 1,2ml; V3 = 1,5ml,
which is then used to calculate the hardness of Mg2+ by using the following
formula:

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B  C 1000  MrMg
Mg 2 (mg )   pengenceran
L Vol.sampel (ml )

and hardness of Mg2+ obtained at V1 = 1440 g / L; V2 = 1152 mg / L; V3 = 1440


mg / L, in order to obtain hardness of Mg2+ on average for the three titration is
equal to 1344 mg / L. Our value can be in the thousands, so that the hardness of
Mg in the water is very high.

IX. Conclusion
1. The hardness of Ca2+ in the sample is 9,6 mg/l. Because the hardness is Ca2+ is less
than 30, the hardness level is low.
2. The hardness of Mg2+ in the sample is 1344 mg/l. Because the hardness is Mg2+ is
more than 150mg/L, the hardness level is high.

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References

Anonim. 2014. Water Hardness (online). http://www.unitedutilities.com/About-your-


water.aspx. Accessed on November 1st, 2014.

Anonim. 2014. Water Hardness (online). http://www.stwater.co.uk/waterhardness.


Accessed on November 1st, 2014.

Amaria, dkk. 2014. Penuntun praktikum kimia lingkungan. Surabaya: UNESA Press.

Basset, J. et al. 1994. Buku Ajar Vogel Kimia Analisis Kuantitatif Anorganik. Edisi 4.
Jakarta: Buku kedokteran EGC.

Day, R.A. Underwood.A.L.1986. Quantitative Analysis. New York: Prentice Hall


(terjemahan oleh A. Hadyana P 1998). Analisis Kimia Kuantitatif (ed. Ke-6)
Jakarta : Erlangga

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Attachment: Photos

(Ca2+ experiment is not attached because we forget to take photos. We’re sorry T_T)

Photos Notes
Sample after added EBT indicator. The
color is pink.

Sample after titared with EDTA solution


the color changed to blue

All the three replication after titrated


with EDTA solution

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