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Experiment 8 Results and Discussion Report:Quantitative Determination of Total Hardness in Drinking Water by Complexometric EDTA Titration

Experiment 8 Results and Discussion Report:Quantitative Determination of Total Hardness in Drinking Water by Complexometric EDTA Titration

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Published by Nathalie Dagmang
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LEAVE A COMMENT IF YOU ARE USING THIS.

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Published by: Nathalie Dagmang on Mar 27, 2011
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1Nathalie DagmangCo-workers: Annjaneth Briones and group 9Group 8Date Performed: January 27, 2011 
Results and Discussion Report 8:Quantitative Determination of Total Hardness in Drinking Water by Complexometric EDTA Titration
The total hardness of water is measured from the amount of calcium and magnesium present inthe water sample. In this experiment, the total hardness was measured using the complexometric EDTAtitration.Ethylenediaminetetraacetic acid, or EDTA, is widely used in titrations of metal cations. It is arelatively feasible complexing agent because it forms 1:1 complexes with metal cations without losing itsproperties and has 6 complexing groups, one on each of the two nitrogens and each of the four carboxylgroups (as shown in Figure 1). Such complexing agents with two or more complexing groups are calledchelating agent and the complex that is forms is called a chelate. Thus, the complexometric EDTAtitration can also be called chelometric titration.Figure 1. Structure of Ethylynediaminetetraacetic acidThe EDTA serves as the ligand, or the lewis base (electron pair donor) while the metal ion to beanalyzed is the lewis acid (electron pair acceptor) of the complex to be formed. The EDTA is representedin this paper as H
4
Y, to clearly see that it is a tetraprotic acid, or an acid that contains four ionizablehydrogens, which are from the four carboxyl groups. The unprotonated ligand Y
4-
is the specie that isaimed to be produced that will form complexes with the metal ions.Because of the polyprotic properties of EDTA, or Ethylenediamine tetraacetic acid, it exhibits thefollowing behavior:
 
 
 

 
 
 
 

 

 
 


 
 

 

 
 


 
 

 

 
 
 
2EDTA is a weak acid so for this experiment, the pH was buffered at 10 with NH
3
-NH
4
Cl toproduce the aimed amount of Y
4-
. The pH value which will yield the highest percentage of Y
4-
is pH 12.However, this causes the solution to be too basic and the cations to form hydroxides, yielding a differentreaction. The pH value of 10 is enough to allow the specie Y
4-
to predominate and react to yield MgY
2-
,HIn
2-
(blue) and H
+
in the final reaction.Figure 2. Structure of tetracarboxylate ion (Y
4-
)This specie shares its six electron pairs with cations like Mg
2+
and forms strong 1:1 complexes orchelates:Figure 3. Structure of MgY
-
chelateIn this experiment, a metal ion indicator was used to indicate the endpoint of the EDTAtitration. It is a compound which forms a colored metal ion complex at some range of pM (where M isthe metal ion), like how acid-base indicators forms a hydrogen ion complex. Eriochrome Black T, orEBT, has a pH range of 6.3 to 11.5, and exhibits the following behavior:

 

  


 

 
 

 

   

 


 
  

 

  

 with red as its acidic color and orange its basic color. Because of this, it becomes useful in titrationsinvolving more than 2 dozens of metal ions which form red complexes at pH 7-11 like those measured inthis experiment (Mg
2+
and Ca
2+
). It is important that the pH is kept above 7 so that HIn
2-
predominatesand reacts with the cations accordingly:


 

 
  
  
[1]


 

 
  
 
[2]
 
3The stabilities of CaIn
-
, MgIn
-
, [Ca-EDTA]
-
and [Mg-EDTA]
-
complexes have different values, withthe following order of decreasing stability:

 
 
 
 Therefore, as EBT is added to the buffered solution containing the Ca
2+
and Mg
2+
ions, [Mg-In]
-
 will form (equation [2]) and the solutions color will turn wine-red. As the solution is titrated with EDTA,the wine-red color stays until it reaches the endpoint, which occurs when equations [3] and [4] arecompleted in order and the EDTA successfully breaks the Mg-In complex, producing blue HIn
2-
ion. Fe
3+
 from the water may bond with the indicator and yield a violet colored solution, instead of the desiredendpoint color blue. After the addition of buffer, KCN can be added so that this bonds with the Fe
3+
andallow the color change to the desired blue.


 

 

[3]


 

 

[4]

 

 
 

 

 
[5]MgY
2-
has a higher formation constant hence a higher tendency to form, than CaY
2-
. Thus,magnesium can kick out calcium from the CaY
2-
complex that formed first and form MgY
2-
complex. Thisis also the reason why MgCl-6H
2
0 crystals are added to the titrant when it is prepared. This is becausethe CaIn complex is not very stable and will be easily affected when EDTA is added, so by adding Mgions, the endpoint will become sharp and will not come too early in the titration. Also, EDTA does notreadily dissolve in water. So, NaOH pellets were added to the solution to convert it into a more solublesalt form. This step also causes the pH to be more basic, allowing the dissolution of EDTA which onlydissolves at pH 8.After the endpoint is detected, the amount of MgY
2-
complex formed will then be calculated,which is also equal to the amount of Calcium ions that it kicked out from its complex. The totalhardness is then calculated as ppm CaCO
3
based on the assumption that all the cations Mg
2+
and Ca
2+
 originated from dissolved CaCO
3
. This was done by calculating the titer CaCO
3
from the standardizationthen multiplying this by the volumes of titrant used in the analysis part of the experiment.In the experiment, the calculated ppm CaCO
3
was 68 ppm with a confidence interval of + 2.Based on the table below, the value of ppm CaCO
3
calculated indicates that the water sample ismoderately hard.Table 1. Water Hardness and ppm CaCO
3
 
Water hardness ppm CaCO
3
 
Soft 0-20Moderately Soft 20-60Moderately Hard 61-120Hard 121-180Very hard >180

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