A. TITTLE Iodometric Titration B. PURPOSE 1. Determine (Standardized) the concentration of Na2S2O3 2. Determine Cl2 in the bleaching powder C.

THEORY The term oxidation refers to any chemical change in the which there is an increase is in oxidation number, while reduction is Used for every Decrease in oxidation. That means the oxidation processes accompanied by the loss of electrons while the electrons gain reduction. Oxidant is a compound contained in the which Atoms decreased oxidation. Instead of reducing agent, the Atoms contained Increased oxidation. Oxidation-reduction Should always take place together and mutually compensate EACH other. The term oxidator and reductor refers to a reductant oxidant compounds, not only to the atomic. Less frequently prescribed Than oxidizing the reductant. However, the oxidant cans be determined with the reductant. That Reductant are commonly Used for the determination of oxidant is potassium iodide, titanium ions (III), iron ion (II), and vanadium ions (II). How redox titration using iodine solution as titrant Called iodimetric, while using a solution of iodide as totran Called iodometric. Iodometry is one of the most important redox titration methods. Iodine reacts directly, fast and quantitively with many organic and inorganic substances. Thanks to its relatively low, pH independent redox potential, and reversibility of the iodine/iodide reaction, iodometry can be used both to determine amount of reducing agents (by direct titration with iodine) and of oxidizing agents (by titration of iodine with thiosulfate). In all cases the same simple and reliable method of end point detection, based on blue starch complex, can be used. Reversible iodine/iodide reaction mentioned above is 2I- I2 + 2eand obviously whether it should be treated as oxidation with iodine or reduction with iodides depends on the other redox system involved.

In the analytic process, iodine is used as an oxidizing reagent (iodimetric) and iodide ions are used as reduction reagent (iodometric). Relatively few substances are quite strong reduction reagent to be titrated directly with iodine. So the number is slightly iodimetrik determination. However, many oxidizing reagents are strong enough to react completely with iodide ions, and there are a lot of use iodometric process. An excess of iodide ion was added to the oxidizing reagent is determined, with the release of iodine, which is then titrated with sodium thiosulfate. The reaction between iodine and thiosulfate in a perfect place. Iodine is only slightly soluble in water (0.00134 moles per liter at 25 0C), but slightly soluble in a solution containing iodide ions. Standard iodine solution can be made by direct weighing and dilution in pure iodine volumetric bottle. Iodine, purified by sublimation and added to a concentrated solution of KI, which weighed carefully before and after adding iodine. But the solution is usually standardized against a primary standard, the most commonly used As2O3. Standard solution used in most iodometric process is sodium thiosulfate. Salt is usually available as pentahidrate Na2S2O3.5H2O. Solution should not be standardized by weighing directly, but must be standardized against primary standard. Sodium thiosulfate is not stable for a long time. A number of solids used as the primary standard to a solution of sodium thiosulfate. Pure iodine is the most obvious standards, but is rarely used because of difficulties in handling and weighing. More frequent use of strong reagents which liberate iodine from iodide, a process iodometric. Second important reaction used excesivelly in iodometry is reduction of iodine with thiosulfate: 2S2O32- + I2 S4O62- + 2IIn the case of both reactions it is better to avoid low pH. Thiosulfate is unstable in the presence of acids, and iodides in low pH can be oxidized by air oxygen to iodine. Both processes can be source of titration errors. Color 0.1 N iodine solution is strong enough so that iodine can work as an indicator itself. Iodine also gives the color purple or violet red to strong solvents as carbon tetrachloride or chloroform and sometimes this is used to determine the titration endpoint. But the more common use of a solution (colloidal dispersion), starch, because the dark

blue color of starch-iodine complex is used for a test is very sensitive to iodine. Greater sensitivity in the solution slightly acidic than neutral solution and larger in the presence of iodide ions. Determination of chlorine in bleaching powder. Bleaching powder consists essentially of a mixture of hypochlorite Ca (OCl) 2 and hydrochloric acid bases CaCl2, Ca (OH) 2.H20: little flower of lime. When the process bleaching powder with hydrochloric acid, chlorine released. OCL- + Cl- + 2H+ Cl2 + H2O Then acidified with sulfuric acid is the OCL-+ 2I-+ 2H+ Cl- + 3I2 + H2O The liberated iodine titrated with sodium thiosulfate standard. ClO3- + 6I- + 6H+ Cl- + 3I2 + 3H2O

D. DESIGN OF EXPERIMENT Equipment / Materials: 1. Calium Iodate 2. Aquadest 3. Na2S2O3 4. KI solution 20% 5. HCL 4N 6. Strach Solution 7. Volumetric Flask 100 mL 8. Erlenmeyer 100 mL 9. Graduated Cylinder 10 mL 10. Stative 11. Burette 12. Volumetric Pipette

13. Pipette 14. Bleaching solution

Procedure 1. Standardization of Na2S2O3 0.3337g of KIO3 - Entered into Volumetric Flask 100 mL - Added water until V= 100 mL - Shaked Standard Solution Pipette 10 mL Entered into Erlenmeyer 100 mL Added 4 mL KI Solution 20% Added 1 mL HCl 4N Titrated with Na2S2O3 three times

Indicator Change Color - Added 2-3 mL Starch solution - Titrated with Na2S2O3 Blue Color Lost

2. Application of Titration of Neutralization 2 mL of Bleaching Solution Measured its density Noted its brand Entered to erlenmeyer 100 mL Added 75 mL Aquadest Added 0.3 grams KI Added 8 mL H2SO4 Added 3 drops Ammonium Molibdat 3% Titrated with Na2S2O3

Change Color

- Added 5 mL starch solution - Titrated with Na2S2O3 Broen Color Lost

E. DATA Treatment Standarization of Na2S2O3 1. Entered 0.3337 g of KIO3 into volumetric flask 2. Dilute until V=100 ml with aquadest 3. Taked KIO3 solution 10 ml into erlenmeyer 4. Added 4 ml of KI 20% 5. Added 12 ml of HCl 4N 6. Titrated with Na2S2O3 Before After

KIO3 : solid, white -aquos, colorless crystal Aquadest : aquos, colorless

KI 20% : aquos, colorless HCl : aquos, colorless Na2S2O3 : aquos, colorless

-aquos, colorless -aquos, raddish brown V1 = 8.6 ml V2 = 8.5 ml V3 = 8.4 ml Color : soft yellow

7. Added amilum 2-3 ml 8. Titrated with Na2S2O3

Amilum colorless

aquos, -dark purple V1 = 0.1 ml V2 = 0.2 ml V3 = 0.3 ml Color : colorless Vtotal = 8.7 ml Vtotal = 8.7 ml Vtotal = 8.7 ml Colorless, aquos

Application 1. Entered 2 ml of bleaching solution bleaching solution : aquos, colorless into erlenmeyer brand : so klin pemutih density : 1.0912 g/ml KI : solid, white crystal 2. Added 75 ml aquadest H2SO4 : aquos, colorless 3. Added 0.3 g of KI Ammonium molibdate : 4. Added 8 ml of H2SO4 2 N 5. Added 3 drops of ammonium aquos, colorless molibdate

Yelow, aquos Dark brown, aquos Dark brown, aquos

6. Titrated with Na2S2O3

7. Added 5 ml ammilum 8. Titrated with Na2S2O3

V1 = 9.4 ml V2 = 9.1 ml V3 = 9.4 ml Color : yellow, dark brown lost, aquos Dark blue V1 = 0.1 ml V2 = 0.2 ml V3 = 0.3 ml Vtotal = 0.1 ml Vtotal = 0.2 ml Vtotal = 0.3 ml Color : colorless, aquos

F. ANALYSIS Making of KIO3 A total of 0.3337 grams KIO3 in the form of white powder into 100 mL volumetric flask. Then added by distilled water (aquadest) which is colorless and sirred until completely dissolved. After that, add more water until the mark limit of 100 mL so obtained the colorless KIO3 0.09356 N. normality values obtained from the formula :

G. Standardization of Na2S2O3 solution with KIO3 as standard From 100mL of KIO3 (colorless) that have been made, taken 10mL by using volumetric pipette then entered into Erlenmeyer then added 4mL of KI 20% (colorless) then added 1mL HCl 4N (colorless). Those adding is to make the acid condition in the solution. From the adding that have been done, obtained the yellowbrown solution then, this solution is titrated with Na2S2O3 (colorless) until the solution become soft pink. Then the solution is added by 4 drops by starch solution (colorless) then the solution become blue. This shows that in I2 solution and in starch solution uses as indicator. The this solution is titrated again until the blue color gone precisely. This shows that in the solution is contain no more I2, but has become I-. This experiment is done three times and obtained volume of Na2S2O3 as follows:

V1 = 8.7 mL, V2 = 8.7 mL , V3 = 8.7 mL. The three experiment obtained the same volume of Na2S2O3. So the calculation is using the formula below :
Equivalence mol KIO3 = equivalence mol Na2S2O3

Because the volume of three experiment are same, so obtained the Na2S2O3 normality is 0.1075 N. Normality that obtained is used for find the data in next experiment. Reaction that happened as follows:

2IO3- + 12H+ + 10e2I2IO3- + 12H+ + 10 I-

I2 + 6H2O I2 + 2e6 I2 + 6H2O

x1 x5

2 S2O32e- + I2 2 S2O3- + I2

S4O62- + 2e2IS4O62- + 2I-

Application of determine the concentration of Cl2 in bleaching solution The percentage of Cl2 in bleaching that sell in public market is has different experiment value. In this experiment, we use So Klin Pemutih. To measure its density of the bleaching we use picnometer. The mass of bleaching that obtained is 27.28 grams, while the volume is 25 mL. So obtained the density of the bleaching is 1.0912 gram/mL. Then it take 2mL and then entered into Erlenmeyer and added 75mL aquadest for not too dense. And the added 0.3 grams KI as white powder so its obtained brown-yellow solution. Then added by 8mL H2SO4 (colorless) that use to make acidic condition is that solution. Then added 3 drops of Amonium molibdat 3% (colorless) as catalyst to make reaction faster. From these adding obtained brown solution and obtained precipitation. Then, it titrated with Na2S2O3 (colorless) until the solution become soft yellow and the precipitation is gone. After become soft yellow, the solution is added by 5mL starch solution (colorless) then the solution become black-blue. It shows that in the solution contain

I2 and the starch solution is use as indicator. Then it titrated again with the blue color is gone precisely. It shows that in this solution contains no more I2 and become I-. This experiment is done three times and obtained volume of Na2S2O3 that used as follows: V1 = 9.5 mL , V2 = 9.3 mL , V3 = 9.5 mL. So the calculation is using the formula below:
Equivalence mol Cl2 = equivalence mol Na2S2O3

Then, to find the percentage of Cl2 is using the formula:

Reaction that happend: Cl2 + 2 I- 2Cl- + I2 I2+ 2 S2O32- S4O62- + 2 IIn the first volume, obtained the equivalence mol of Cl2 is 1.02125 x 10-3. So known that mass Cl2 is 36.25 x 10-3 gram and the percentage of Cl2 is 1.6610 %. In the second volume, obtained the equivalence mol of Cl2 is 0.99975 x 10-3. So known that mass Cl2 is 0.0354 gram and the percentage of Cl2 is 1.6262 %. In the third volume the value is same with second value because has the same volume. So, the average percentage of Cl2 is.

H. DISCUSSION When first titrated In Na2S2O3 standardization the color of yellow become colorless because we late to stop the burette.

I. CONCLUSION 1. The Normality of KIO3 as standard solution is 0.09356 N. Then the Normality Na2S2O3 solution is 0.1075 N. 2. For the Iodometri application, obtained the percentage Cl2 in bleaching solution is 1.6494 %. J. QUESTION OXIDIMETRI TITRATIONI A. 1. Fe2+ Fe3+ + e (reduktor) (oksidator) MnO4- + 8H+ + 5e Mn2+ + 4H2O 1mol Fe2+ 1 eqivalen MnO42. For the potential system Fe2+ Fe3+ in the titration vessel can be measured at any point in making this vessel a half galvanic standard. A slow platinum electrodes used in indicator. B. 1. Iodometri : - I- as reductor - Reaction : sample + I- I2 + .
-

5Fe2+ + MnO4- + 8H+ 5Fe3+ + Mn2+ + 4H2O

cell. Another is

the electrode half-cell electrode

the titration vessel as an

I2 that formed reaction with S2O32-

- S2O32- standarisation with K2Cr2O7 / KIO3 Iodimetri : - I2 as oxidator - Reaction : sample + I2 I- + . - Indikator amilum. Amilum + I2 purpish blue Amilum + I- colorless S2O32- standarisation with HAsO2 2I I2 + 2e

2. 2IO3- + 12H+ + 10e I2 + 6H2O 2IO3- + 12H+ + 10I- 6I2 + 6H2O every 1 mol KIO3 = 5 eqivalent

APPLICATION IODI-IODOMETRIC TITRATION 1. (i) are non-soluble in cold water; (ii) instability suspension in water; (iii) with iodine to give a complex which can not dissolve in water, so that the starch should not be added too early in the titration. (therefore, the iodine titration, starch solution should not be added until just before the end point, when the colors start to fade) and (iv) there is sometimes the end point of the 'float', a striking when a dilute solution. 2. Because if added at the beginning of iodine to give a complex which can not dissolve in water 3. To prevent excessive carbon dioxide, this can cause slow decomposition accompanied by the formation of sulfur: S2O3- + H+ HSO3- + S

Moreover, the decomposition can also be caused by bacteria work (eg, thiobacilusthioparus), especially if the solution has been silenced for some time.

K. REFFERENCES Basset, J. et al. 1994. Buku Ajar Vogel Kimia Analisis Kuantitatif Anorganik. Edisi 4. Jakarta: Buku kedokteran EGC. Day, R. A, and Underwood. A.L. 2002. Analisis Kimia Kuantitatif. Edisi ke-6. Jakarta: Erlangga. Poedjiastoeti, Sri. dkk. 2007. Panduan Praktikum Dasar Dasar Kimia Analitik. Surabaya: Jurusan Kimia FMIPA Universitas Negeri Surabaya.

ATTACHMENT Reaction : 2 IO3- + 12 H+ + 10 e I2 + 6 H2O 2I I2 + 2e 2 IO3 + 10 I- +12 H+ 6 I2 + 6 H2O I2 + 2e 2 S2O322 S2O32- + I2

2I-

x1 x5

S4O62- + 2e S4O62- + 2I-

Known : mass of IO3- = 0.3337 gram V1of S2O32- = V2of S2O32- = V3of S2O32- = 8.7 ml n=6 volume of IO3- = 100 ml Mr = 214

0.3337 g of KIO3

Na2S2O3

100 ml

Taked 10 ml into erlenmeyer

4 ml of KI 20 % 1 ml of HCl 4N

Answer : Eq of IO3- = m x n BE = 0.3337 x 6 214 = 9.35607 x 10-3 mol eq N of IO3- = eq V = 9.35607 x 10-3 mol eq 0.1 L = 9.35607 x 10-2 mol eq = 0.09356 N Mol eq of IO3V1 x N1 10 ml x 0.09356 N N2 = mol eq S2O32= V2 x N2 = 8.7 ml x N2 = 0.9356 8.7 = 0.1075 N Because the volume of S2O32- is same, so the average normality is 0.1075 N.

Application : Cl2 + 2I- 2Cl- + I2 I2 + 2 S2O32- S4O62- + 2IV1 of Cl2 = 9.5 ml V2 of Cl2 = 9.3 ml V3 of Cl2 = 9.5 ml Mass of sample = V sample x sample = 2 ml x 1.0912 gram/ml = 2.1824 gram mol eq Na2S2O3 V1 Na2S2O3 x N Na2S2O3 mol eq Cl2 = mol eq Cl2 = mol eq Cl2 = 0.1075 N x 9.5 ml = 1.02125 x 10-3

mass of Cl2 % Cl2

= 1.02125 x 10-3 x 35.5 = 36.25 x 10-3 gram = 36.25 x 10-3 gram x 100 % 2.1824 gram = 1.66 %

mol eq Na2S2O3 V2 Na2S2O3 x N Na2S2O3 mol eq Cl2 mass of Cl2 % Cl2

= mol eq Cl2 = mol eq Cl2 = 0.1075 N x 9.3 ml = 0.99975 x 10-3 = 0.99975 x 10-3 x 35.5 = 35.4 x 10-3 gram = 35.4 x 10-3 gram x 100 % 2.1824 gram = 1.6262 %

V3 = V1, so % of Cl2 in V3 = V1 Average of % Cl2 = 1.66 % + 1.6262 % + 1.66 % 3 = 1.648 %