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Experiment 5 - Oxidation-Reduction Titration Iodimetry

Experiment 5 - Oxidation-Reduction Titration Iodimetry

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Published by: Alma Pabilane on Jun 16, 2012
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Experiment 5: Oxidation Reduction Titration Iodimetry
dela Cruz, Marie Giecel V.Pabilane, Alma L.Group 6, Chem 27.1, SEJ1, Ms. Noime WalicanJanuary 29, 2011
I. Abstract
Iodimetry is an oxidation-reduction titration which uses iodine, an oxidizing agent that reacts rapidly with avariety of strong reductants, as titrant, with starch as the indicator. On the other hand, iodometry is a redox titrationwherein I
2
is being produced in the system. Iodometric methods are used in the determination of many organic andinorganic substances, with Na
2
S
2
O
3
as titrant (commonly used). The concentrations may be expressed as %(w/w)of the ion or metal desired. This amount of I
2
present can be calculated by the stoichiometry of the titrant used withI
2
according to the balanced redox reaction. Then, the amount of the desired ion or metal will be computed usingthe ratio of this ion with I
2
according to the balanced reaction. In this experiment, iodometric method is done todetermine the bleaching power (which is the concentration of Cl
-
) of a bleach. The experimental result for theconcentration of Cl
-
in the sample bleach was 1.788x10
-4
g/ml.
II. Keywords:
iodometry, iodimetry, redox titrations, oxidant, reductant
III. Objectives
In this experiment, the students must be able to:(1)Prepare a standard solution of Na
2
S
2
O
3
and;(2)Determine the strength of bleachingagent by oxidation – reduction titration.
IV. Introduction and Principles
Oxidation – reduction titrations involves thetitration between an oxidizing agent and a reducingagent.Iodimetry is a redox titration that uses iodineas the titrant. Although iodine’s oxidizing power isless than that of ceric, permanganate and dichromateions, it is widely used as redox titrant because of itsability to react rapidly with many strong reductants,and the availability of a good indicator for iodinewhich is starch. Starch forms a deep-blue complexwith iodine, but not with iodide. The half reaction for the reduction of iodine is given by:I
2(s)
+ 2e
-
 

2I
-
 Iodine also has some disadvantages. It is notvery soluble in water but dissolves readily in an iodidesolution forming triiodide ion. Also, iodine solutionsare not very stable. It can be oxidized by oxygen inacidic medium.Iodometry, which is the one performed in thisexperiment, uses iodide ion, not as titrant, but to
 produce
iodine in the system. Then, the iodine isconsumed in the titration. The reagent most oftenused as titrant for iodine is sodium thiosulfate(Na
2
S
2
O
3
). Its reaction with iodine is given by:I
2
+ S
2
O
32-
 

2I
-
+ S
4
O
62-
Thiosulfate ion is a moderately strongreductant. It is readily soluble in water and is stable inboth neutral and basic conditions. It is one of the fewreducing agents that are not oxidized by air. It hasbeen widely used to determine oxidizing agents by anindirect procedure, involving iodine as intermediate.The scheme used to determine the oxidizing agentsinvolves addition of excess KI to slightly acidicanalyte. The reduction of the analyte produces astoichiometrically equivalent amount of iodine, andthen the produced iodine is titrated with standardsolution of sodium thiosulfate as indicated in thereaction above.Redox titration curve is a plot of electrodepotential vs. volume of titrant used. The electrodepotential is a log function of the concentration of titration of reactants and products and it refers to thepotential of the electrode immersed in the solutionrelative to standard hydrogen electrode.
V. Methodology and Materials
 A. Preparation and Standardization of 0.1MNa
2
S
2
O
3
solutionThe weight of Na
2
S
2
O
3
(H
2
O)
5
crystals needed toprepare 500ml of 0.1M Na
2
S
2
O
3
solution wascalculated. This amount of crystal was dissolved in100ml previously boiled distilled water in a beaker. Itwas diluted to 500ml and 0.20g sodium carbonatewas added as preservative. The solution was storedin a clean reagent bottle.In each of the three 500-ml Erlenmeyer flasks,0.10-0.15 g of primary standard grade potassiumdichromate was placed. Each sample was dissolvedin 50ml previously boiled distilled water and 4ml of 1:2 sulfuric acid was added. Five grams of KIdissolved in 5ml distilled water was added and theflask was swirled. The flask was covered with watchglass and allowed to stand for 3 minutes to allow thereaction to complete.Chem 27.1. Oxidation Reduction Titration Iodimetry Page
1
of 
3
 
The solution was diluted with 50ml double-distilled water and titrated with thiosulfate solutionuntil the brown color of iodine had almostdisappeared. Five milliliters of starch solution(prepared in procedure B) was added and titrationwas continued until the last drop of titrant removedthe blue color of starch iodine complex giving a clear emerald-green solution.Three trials were done and the molarity of sodium thiosulfate was calculated in each. Theaverage deviation should be 1-3ppt.B. Preparation of Starch Indicator In 5ml double-distilled water, 0.5 g starchwas dissolved. This was added to 100ml boiling water and was boiled for another 2 minutes.C. Analysis of the UnknownFifty milliliters of liquid bleach was placed in a250-ml volumetric flask and was diluted to mark. Tenmilliliters of this was put in each of the five 250-mlErlenmeyer flasks. Then, 50ml of distilled water wasadded to it. Three grams KI, 8ml of 1:6 sulfuric acidand 3 drops of 3% ammonium molybdate (catalyst)were added. The flasks were covered with watchglass and let stand for 3 minutes to allow reaction tocomplete. The liberated iodine was titrated withstandardized thiosulfate solution until brown color of iodine has almost disappeared. Five milliliters of starch indicator was added and titration wascontinued until blue color disappeared.The % Cl in each trial was calculate,assuming the density of liquid bleaches is 1.0 g/mol.
VI. Results
Reactions Involved:Standardization14H
+(aq)
+ Cr 
2
O
72-(aq)
+ 6I
-(aq)
 
2Cr 
3+(aq)
+ 3I
2(aq)
+ 7H
2
O
(l)
2S
2
O
32-(aq)
+ I
2(aq)
 
2I
-(aq)
+ S
4
O
62-(aq)
Bleaching power 2S
2
O
32-(aq)
+ I
2(aq)
 
2I
-(aq)
+ S
4
O
62-(aq)
2H
+(aq)
+ ClO
-(aq)
+ 2I
-(aq)
I
2(aq)
+ Cl
-(aq)
+ H
2
O
(l)
A.
Standardization of Na
2
S
2
O
3
TrialW,K
2
Cr 
2
O
7
(g)V,Na
2
S
2
O
3
(mL)M,Na
2
S
2
O
3
(M)10.109513.830.161520.102413.480.154930.102513.270.1575 Ave = 0.1580 MComputations:1: [(0.1095 g K
2
Cr 
2
O
7
/ 294.19 g/mol)(mol Cr 
2
O
72-
/mol K
2
Cr 
2
O
7
)(3 mol I
2
/ mol Cr 
2
O
72-
)(2 mol S
2
O
32-
/ 1mol I
2
)] / (0.01383 L) = 0.1615 M2: [(0.1024 g K
2
Cr 
2
O
7
/ 294.19 g/mol)(mol Cr 
2
O
72-
/mol K
2
Cr 
2
O
7
)(3 mol I
2
/ mol Cr 
2
O
72-
)(2 mol S
2
O
32-
/ 1mol I
2
)] / (0.01348 L) = 0.1549 M3: [(0.1025 g K
2
Cr 
2
O
7
/ 294.19 g/mol)(mol Cr 
2
O
72-
/mol K
2
Cr 
2
O
7
)(3 mol I
2
/ mol Cr 
2
O
72-
)(2 mol S
2
O
32-
/ 1mol I
2
)] / (0.01327 L) = 0.1575 MB.Determination of Bleaching Power TrialV, Na
2
S
2
O
3
(mL)% Cl
-
(g/mL)115.751.764x10
-4
216.31.826x10
-4
316.151.809x10
-4
415.811.771x10
-4
515.81.770x10
-4
 Ave = 1.788 x 10
-4
g/mLComputations:n, S
2
O
32-
1: n, S
2
O
32-
= (0.1580 M)(0.01575 L) = 2.4885 x 10
-3
mol2: n, S
2
O
32-
= (0.1580 M)(0.01630 L) = 2.5754 x 10
-3
mol3: n, S
2
O
32-
= (0.1580 M)(0.01615 L) = 2.5517 x 10
-3
mol4: n, S
2
O
32-
= (0.1580 M)(0.01581 L) = 2.49798 x 10
-3
mol5: n, S
2
O
32-
= (0.1580 M)(0.01580 L) = 2.4964 x 10
-3
molM, ClO
-
1: M ClO
-
= [(2.4885 x 10
-3
mol S
2
O
32-
)(mol I
2
/ molS
2
O
32-
)(mol ClO
-
/ mol I
2
)] / [(0.010 L)(250 mL / 10mL)]= 4.977 x 10
-3
M2: M ClO
-
= [(2.5754 x 10
-3
mol S
2
O
32-
)(mol I
2
/ molS
2
O
32-
)(mol ClO
-
/ mol I
2
)] / [(0.010 L)(250 mL / 10mL)]= 5.1508 x 10
-3
M3: M ClO
-
= [(2.5517 x 10
-3
mol S
2
O
32-
)(mol I
2
/ molS
2
O
32-
)(mol ClO
-
/ mol I
2
)] / [(0.010 L)(250 mL / 10mL)]= 5.1034 x 10
-3
MChem 27.1. Oxidation Reduction Titration Iodimetry Page
2
of 
3

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