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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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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
Pink solution
Volume of
EDTA solution
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1 ml sample
25 ml diluted sample
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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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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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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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
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:
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 )
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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:
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 )
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
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.
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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.
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