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Complexometric titration



Complexometric titration  :
(sometimes chelatometry)
                    is a form of volumetric analysis in which the formation of a colored complex is used to indicate the end point of a titration. Complexometric titrations are particularly useful for the determination of a mixture of different metal ions in solution. An indicatorcapable of producing an unambiguous color change is usually used to detect the end-point of the titration.when is the complexometric titration is know as chelatometry titration.

Complexometric Titration or chelatometry is a type of volumetric analysis wherein colored complex is used to determine the endpoint of the titration. Titration is one of the common method used in laboratories which determines the unknown concentration of an analyte that has been identified. It is a method used in the quantitative chemical analysis.
It is sometimes termed as volumetric analysis as measurements of volume play a vital role. Here reagent is used as a standard solution, and they are called titrant. Titrant Volume is defined as the volume of a titrant that is reacted.
Complexometric Titration is in the detection of mixtures of different metal ions present in the solution.

Complexometric Titration Reactions
When each drop of titrant is added, the reaction reaches an equilibrium state swiftly. There would be no chance for any interfering situations. The equivalent point can be identified very accurately using a complexometric titration. EDTA is used as a titrant and it is pretty much well established.

EDTA Complexometric Titration :
EDTA called as ethylenediaminetetraacetic acid is a complexometric indicator consisting of 2 amino groups and four carboxyl groups called as Lewis bases.Edta is a hexadentate ligand because of its competence of to denote six pair of lonely electrons due to the formation of covalent bonds.Even the presence of small metal ions would lead to a distinct change in the color. This leads to the formation of a weak complex.Complexing agents are less soluble in water, and most of them are free acids.They are used in volumetric Solutions. Before using them, they are converted into sodium salts that are feasible in water.Since they are characterised with less solubility in water, they are used for titration.Sometimes simple titration methods are used to determine the simple metal ions present in water. But to determine the exact number of metal ions present complexometric titration is used, and it is conducted using EDTA.

masking agent is a reagent used in chemical analysis which reacts with chemical species that may interfere in the analysis.
In sports a masking agent is used to hide or prevent detection of a banned substance or illegal drug like anabolic steroids or stimulants. Diuretics are the simplest form of masking agent and work by enhancing water loss via urine excretion and thus diluting the urine, which results in lower concentrations of the banned substance as more of it is being excreted from the body making it more difficult for laboratories to detect.

Demasking is the technique of releasing the masked species so that it is free to react with the principal reagent. Demasking is thus used to offset the effect of a masking agent.

Estimation of calcium gluconate :

Calcium can be determined by EDTA titration in solution of 0.1 M sodium hydroxide (pH 12-13) against murexide. Just like during determination of magnesium all metals other than alkali metals can interfere and should be removed prior to titration. Magnesium in that high pH precipitates as Mg(OH)2 and is not complexed by EDTA, thus its presence can be ignored. Note, that if the amount of magnesium is huge, calcium can coprecipitate with Mg(OH)2. Presence of ammonium salts is undesired, as they lower pH and make end point less sharp. To get rid of ammonia, solution can be heated after NaOH was added.

reaction
Reaction taking place during titration is
Ca2+ + EDTA4- → CaEDTA2-

sample size
For 0.01 M titrant and assuming 50 mL burette, aliquot taken for titration should contain about 0.35-0.45 millimoles of calcium (14-18 mg). If preparation of such sample is difficult, we can use different EDTA concentration.

end point detection
End point of calcium titration is easily detected with murexide, assuming pH is high enough. Murexide solutions are not stable and should be not stored longer than a week.

solutions used
To perform titration we will need titrant - 0.01 M EDTA solution and 1 M sodium hydroxide solution. We will also need indicator - either in the form of solution, or ground with NaCl - 100 mg of indicator plus 20 g of analytical grade NaCl.

procedure
Procedure to follow is mostly identical with the one used for the EDTA standardization.
Transfer calcium solution to Erlenmeyer flask.Dilute to about 100 mL with distilled water.Add 10 mL of 1 M sodium hydroxide solution.Add a pinch of murexide ground with sodium chloride (100 mg of indicator plus 20 g of analytical grade NaCl).Titrate with EDTA solution till the color changes to violet.

result calculation:
Calculation of EDTA titration results is always easy, as EDTA reacts with all metal ions in 1:1 ratio:
Ca2+ + EDTA4- → CaEDTA2-
That means number of moles of calcium is exactly that of number of moles of EDTA used.

sources of errors
In general this is a simple titration, with no other problems then those listed as general sources of titration errors. In the presence of huge amounts of magnesium there is a risk that some calcium will precipitate together with Mg(OH)2, thus introducing negative error to the titration result.

Estimation of Magnesium sulphate :

general remarks
Magnesium can be easily determined by EDTA titration in the pH 10 against Eriochrome Black T. If the solution initially contains also different metal ions, they should be removed or masked, as EDTA react easily with most cations (with the exception of alkali metals). Calcium can be precipitated as carbonate or oxalate, although presence of oxalates may make end point detection difficult.

reaction
Reaction taking place during titration is
Mg2+ + EDTA4- → MgEDTA2-
sample size
For 0.01 M titrant and assuming 50 mL burette, aliquot taken for titration should contain about 0.35-0.45 millimoles of magnesium (8.5-11 mg). If preparation of such sample is difficult, we can use different EDTA concentration.

end point detection
End point of magnesium titration is easily detected with Eriochrome Black T.
solutions used
To perform titration we will need titrant - 0.01 M EDTA solution and ammonia pH 10.0 buffer. We will also need indicator - either in the form of solution, or ground with NaCl - 100 mg of indicator plus 20 g of analytical grade NaCl.

procedure
Procedure to follow doesn't differ much from the one used for the EDTA standardization.
Transfer magnesium solution to Erlenmeyer flask.Dilute to about 100 mL with distilled water.Add 2 mL of pH 10 ammonia buffersolution.Add a pinch of Eriochrome Black T ground with sodium chloride (100 mg of indicator plus 20 g of analytical grade NaCl).Titrate with EDTA solution till the color changes to blue.

result calculation
Calculation of EDTA titration results is always easy, as EDTA reacts with all metal ions in 1:1 ratio:
Mg2+ + EDTA4- → MgEDTA2-
That means number of moles of magnesium is exactly that of number of moles of EDTA used.
sources of errors

In general this is a simple titration, with no other problems then those listed as general sources of titration errors. The most likely problem is spotting the end point, which is not always sharp.
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