coef distribution iod

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Fractional Distillation Page 1 I. EXPERIMENT TITLE : Distribution Coefficient of Iod II. EXPERIMENT DATE : May 4 th , 2015 at 7.30 p.m III. END OF THE EXPERIMENT : May 4 th , 2015 at 10.30p.m IV. EXPERIMENT PURPOSE : - Extraction Iodium into organic solvent - Calculate the distribution coefficient of Iod V. BASIC THEORY A. Extraction Crystallization, purification, and isolation (may only be restricted to a solid) are insufficient ways to separate mixtures of compounds. Extraction is the recovery of a substance from a mixture by bringing it into contact with a solvent, which dissolves the desired material. Partitioning is the separation between two distinct phases (immiscible liquids) and also called fractional separation. Like recrystallization and distillation, extraction is a separation technique frequently employed in the laboratory to isolate one or more components from a mixture. Unlike recrystallization and distillation, it does not yield a pure product; thus, the former techniques may be required to purify a product isolated by extraction. In the technical sense extraction is based on the principle of the equilibrium distribution of a substance (solute) between two immiscible phases, one of which is usually a solvent. The solvent need not be a pure liquid but may be a mixture of several solvents or a solution of some chemical reagent that will react with one or more components of the mixture being extracted to form a new substance soluble in the solution. The material being extracted may be a liquid, a solid, or a mixture of these. Extraction is a very general, highly versatile technique that is of great value not only in the laboratory but also in everyday life. Extraction is a convenient method for separating an organic substance from a mixture, such as an aqueous reaction mixture or a steam distillate. The extraction solvent is usually a volatile organic liquid that can be removed by evaporation after the desired component has been extracted. The extraction technique is based on the fact that if a substance is insoluble to some extent in two immiscible liquids, it can be transferred from one liquid to the other by shaking it together with the two liquids. For example, acetanilide is partly soluble in both water and ethyl ether. If a solution of acetanilide in water is shaken with a portion of ethyl ether (which is immiscible with water), some of the

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Koefisien distribusi Iod Laporan praktikum kimia analitik II universitas negeri surabaya

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  • Fractional Distillation Page 1

    I. EXPERIMENT TITLE : Distribution Coefficient of Iod

    II. EXPERIMENT DATE : May 4th , 2015 at 7.30 p.m

    III. END OF THE EXPERIMENT : May 4th , 2015 at 10.30p.m

    IV. EXPERIMENT PURPOSE :

    - Extraction Iodium into organic solvent

    - Calculate the distribution coefficient of Iod

    V. BASIC THEORY

    A. Extraction

    Crystallization, purification, and isolation (may only be restricted to a solid)

    are insufficient ways to separate mixtures of compounds. Extraction is the recovery

    of a substance from a mixture by bringing it into contact with a solvent, which

    dissolves the desired material. Partitioning is the separation between two distinct

    phases (immiscible liquids) and also called fractional separation.

    Like recrystallization and distillation, extraction is a separation technique

    frequently employed in the laboratory to isolate one or more components from a

    mixture. Unlike recrystallization and distillation, it does not yield a pure product;

    thus, the former techniques may be required to purify a product isolated by

    extraction. In the technical sense extraction is based on the principle of the

    equilibrium distribution of a substance (solute) between two immiscible phases, one

    of which is usually a solvent. The solvent need not be a pure liquid but may be a

    mixture of several solvents or a solution of some chemical reagent that will react

    with one or more components of the mixture being extracted to form a new

    substance soluble in the solution. The material being extracted may be a liquid, a

    solid, or a mixture of these. Extraction is a very general, highly versatile technique

    that is of great value not only in the laboratory but also in everyday life. Extraction

    is a convenient method for separating an organic substance from a mixture, such as

    an aqueous reaction mixture or a steam distillate. The extraction solvent is usually a

    volatile organic liquid that can be removed by evaporation after the desired

    component has been extracted.

    The extraction technique is based on the fact that if a substance is insoluble

    to some extent in two immiscible liquids, it can be transferred from one liquid to the

    other by shaking it together with the two liquids. For example, acetanilide is partly

    soluble in both water and ethyl ether. If a solution of acetanilide in water is shaken

    with a portion of ethyl ether (which is immiscible with water), some of the

  • Fractional Distillation Page 2

    acetanilide will be transferred to the ether layer. The ether layer, being less dense

    than water, separates out above the water layer and can be removed and replaced

    with another portion of ether. When this in turn is shaken with the aqueous solution,

    more acetanilide passes into the new ether layer. This new layer can be removed and

    combined with the first. By repeating this process enough times, virtually all of the

    acetanilide can be transferred from the water to the ether.

    As we stated above, the substance being extracted may be a solid.

    Extractions of this type will not be conducted here, but they are probably already a

    part of your own experience. The brewing of tea from tea leaves (or the tea bag that

    combines extraction and filtration) and of coffee from the ground bean are excellent

    examples of the extraction of a solid mixture with a hot solvent (water).

    B. Coefficient Distribution (KD)

    In the laboratory one of the more important applications of the extraction

    process has been its use to remove an organic compound from a solution when

    distillation is not feasible. Extraction is accomplished by shaking the solution in a

    separatory funnel with a second solvent that is immiscible with the one in which the

    compound is dissolved, but dissolves the compound more readily. Two liquid layers

    are formed, and the layer that has most of the desired product in it can be separated

    from the other. Sometimes not the entire product is extracted in a single operation

    and the process must be repeated once or twice more to assure a clean separation. It

    has been found that when two immiscible solvents are shaken together, the solute

    distributes itself between them in a ratio roughly proportional to its solubility in

    each. The ratio of the concentration of the solute in each solvent at equilibrium is a

    constant called the distribution ratio(d) or partition coefficient (K ).

    The larger the value of Kd, the more solute will be transferred to the ether

    with each extraction, and the fewer portions of ether will be required for essentially

    complete removal of the solute.

    [ ]

    [ ] =

    =

    ,where o and aq refer to the organic (ether) and aqueous layers, respectively,

    and Wo and Waq are the weights in grams of material dissolved in each respective

    layer. Co = concentration of organic solution and Caq = concentration of aqueous

    solution.

  • Fractional Distillation Page 3

    C. Separatory Funnel

    A separatory funnel is used to separate immiscible liquids. When two

    immiscible liquids are placed in a separatory funnel, two layers are seen. The denser

    solvent will be the bottom layer. Most halogenated solvents are denser than water,

    most non-halogenated solvents are less dense than water. If you are not sure which

    layer is which, add a drop of water and see which layer it joins.

    The following is an example in which iodine (I2) in being extracted from an

    aqueous solution into dichloromethane (methylene chloride). Iodine, while slightly

    soluble in aqueous solutions, is more soluble in dichloromethane. Therefore, when

    aqueous solution containing iodine is placed in contact with dichloromethane, the

    iodine migrates into (is extracted by) the dichloromethane layer. Iodine in an aqueous

    solution appears brown. Dichloromethane is a colorless liquid. Since dichloromethane

    is a volatile solvent, this extraction should be done in a hood. The performing is

    shown below:

    The aqueous iodine solution (the solution

    to be extracted) and dichloromethane

    poured.

    A portion of the dichloromethane is

    added to the sep funnel and the funnel

    shaken gently.

  • Fractional Distillation Page 4

    Most of the iodine has been extracted into

    the dichloromethane, the aqueous layer

    becomes lighter brown. The iodine in the

    dichloromethane layer makes it appear

    purplish.

    Remove the stopper and drain the lower

    layer (the dichloromethane layer in this

    case) through the stopcock into a beaker

    or flask. The upper layer should remain in

    the sep funnel.

    The dichloromethane now contains

    almost all the iodine, while only a small

    amount of I2 remains in the aqueous

    layer.

    D. Titration

    Iodine in water solutions is usually colored strong enough so that its presence can be

    detected visually. However, close to the end point, when the iodine concentration is

    very low, its yellowish color is very pale and can be easily overlooked. Thus for the

    end point detection starch solutions are used. Iodine gets adsorbed on the starch

    molecule surface and product of adsorption has strong, blue color. Exact mechanism

    behind adsorption and color change is not known, see for example this explanation of

    starch as an indicator usage. In the presence of small amounts of iodine adsorption

    and desorption are fast and reversible. However, when the concentration of iodine is

    high, it gets bonded with starch relatively strong, and desorption becomes slow, which

    makes detection of the end point relatively difficult. Luckily high concentrations of

    iodine are easily visible, so if we are using thiosulfate to titrate solution that initially

  • Fractional Distillation Page 5

    contains high iodine concentration, we can titrate till the solution gets pale and add

    starch close to the end point. In the case of titration with iodine solution we can add

    starch at the very beginning, as high iodine concentrations are not possible before we

    are long past the end point. At the elevated temperatures adsorption of the iodine on

    the starch surface decreases, so titrations should be done in the cold.

    VI. TOOLS AND MATERIALS

    A. Tools

    Measuring glass

    Volumetric flask

    Erlenmeyer flask

    Burette

    Clamp

    Separated funnel

    Beaker glass

    Pipette

    B. Materials

    Iodium 0,1 M

    Chloroform p.a

    Starch solution

    H2SO4(aq)

    Aquades

    Na2S2O3 0,01M

    (c) Adding starch forms the deep purple starchI3

    complex. (d) As the titration continues, the end point

    is a sharp transition from a purple to a colorless

    solution. The change in color from (c) to (d) typically

    takes 12 drops of titrant.

  • Fractional Distillation Page 6

    VII. FLOW CHART

    I.

    II.

    10 mL Iodium 0,01 M

    100 mL Iodium

    -Put into volumetric flask

    Solute with water until

    Volume was 100 mL

    Organic layers Water layers

    10 mL Iodium

    Forming two layers

    -Move into separated funnel

    -Added 5mL CH3Cl(aq)

    -Shake a few minutes

    Separated

  • Fractional Distillation Page 7

    III.

    KD Iod

    -Determine initial

    concentration of Iodium

    - Repeat three times

    Water layers

    Blue color disappear

    -Move into Erlenmeyer

    -Added 4 mL of H2SO4 2M

    -Titrate with Na2S2O3 0,001M

  • Fractional Distillation Page 8

    VIII. DATA OF EXPERIMENT

    No. Procedure Data of Experiment Hypothesis/Rea

    ctions Conclusion

    Before After

    1.

    I2 =

    yellowish

    brown

    Water =

    colorless

    CH3Cl =

    colorless

    I2+water = yellowish

    brown

    I2+CH3Cl two

    layer = orangish

    brown

    Bottom layer = purple

    I2 and CH3Cl is

    non polar

    solution, non-

    polar and non-

    polar, like

    dissolve like

    Reaction

    I2+H2O

    3I2(aq) +

    2CH3Cl(aq)

    2CH3I3(aq)

    +3Cl2(aq)

    Iodine can

    extract in

    organic solvent,

    namely

    chloroform.

    That proven by

    two layer

    (water layer-

    upper layer, and

    organic layer-

    bottom layer )

    2.

    10 mL Iodium 0,01 M

    100 mL Iodium

    -Put into volumetric flask

    Solute with water until Volume was 100 mL

    Organic layers Water layers

    10 mL Iodium

    Forming two layers

    -Move into separated funnel

    -Added 5mL CH3Cl(aq)

    -Shake a few minutes

    -Repeat 2-5 times

    Separated

  • Fractional Distillation Page 9

    3.

    Water layer

    = orangish

    brown

    H2SO4 =

    colorless

    Na2S2O3 =

    colorless

    Starch

    solution =

    colorless

    water layer + H2SO4 +

    starch solution

    blackish purple

    water layer + H2SO4

    + starch solution +

    Na2S2O3 colorless

    Volume Na2S2O3

    needed =

    V1 = 3,7 mL

    V2= 3,8 mL

    V3 = 3,5 mL

    Kd first titration =

    2,86

    KD first titration =

    2,86

    KD second titration =

    3,14

    KD third titration =

    3,14

    KD average =

    I2+ 2e - 2I-

    2S2O32-

    S4O6+ 4e-

    2I2 + 2S2O32-

    4I

    - + S4O6

    Coefficient

    distribution

    Iodine (KD) is 3

    KD Iod

    -Determine initial

    concentration of Iodium

    - Repeat three times

    Water layers

    Blue color disappear

    -Move into Erlenmeyer

    -Added 4 mL of H2SO4 2M

    -Titrate with Na2S2O3 0,001M

  • Fractional Distillation Page 10

    IX. EXPLANATION

    This experiment is have purpose to extract iodine in organic solvent. First, is to

    determine mole of iodine as of standard solutions. In determining mole iodine standard

    solution , the first step that done is take 10 mL of iodine solution 0,1 M reddish brown ,

    then the solution diluted with aquadest use volumetric flask 100 mL and have result

    reddish brown color solution.The reaction that occur is

    I2(aq) + H2O(l) no reaction occur

    After a solution of iodine obtained, the results of dilution is taken as many as 10

    mL using volumetric pippette and then in put into erlenmeyer .After that added 2 mL

    H2SO4 2M that will make change color become brownish orange. The role of H2SO4

    added is because in iodometric titrations are carried out in strongly acid media, a situation

    that promotes the reaction between oxidizing agents and iodide, and also H2SO4 is a

    strong acid and will deliver H+ which will help to proceed the reaction much faster or as a

    catalyst. Then added 1 mL starch solution 2 % , and undergo a change colors become

    purpleish black. Starch solution is added as an indicators for titration, when starch is

    mixed with iodine in water, an intensely colored starch/iodine complex is formed. Many

    of the details of the reaction are still unknown. The iodine/starch complex has energy

    level spacings that are just so for absorbing visible light- giving the complex its intense

    blue color. The complex is very useful for indicating redox titrations, when there is

    excess oxidizing agent, the complex is blue; when there is excess reducing agent, the I5-

    breaks up into iodine and iodide and the color disappears. After that a solution is titrate

    using Na2S2O3 0,01 M . The reaction that occur is

    I2 + 2e- 2I-

    2 S2O3 2-

    S4O62-

    + 2e-

    I2 + 2 S2O3 2-

    2I- + S4O6 2-

    Based on the theory, the end point of I2 is changing color became colorless. From

    theory we know that the color is shown in the picture below (left picture) and our

    experiment (right picture). We can assume that based on the theory our end point is right.

  • Fractional Distillation Page 11

    In this titration, obtained changing color solution become colorless at the volume

    of titrant Na2S2O3 is 9 mL. By knowing the volume of Na2S2O3 that needed , it can use to

    find out a mole from I2 by calculation below:

    Based on the calculation mole Iodine as standard is 0,045 mmol. Which will be

    used to acquire mmol I2 organic in phase, to determine coefficient distribution of Iodine.

    Second steps is to extract iodine, by using a water solvents and organic solvents

    that in this experiment using chloroform . Using chloroform to extract because, iodine is

    a non-polar molecule this has a weak interaction with the hydrogen bonded water

    molecules. The energy associated with the iodine/ water interactions is not enough to

    compensate for the lost energy of the water/water interactions. This ultimately means that

    not much iodine will dissolve in water. If a solvent with weaker solvent/solvent

    interactions than water were introduced to this system, iodine would find it easier to

    disrupt these interactions and insert itself (dissolve) between the solvent molecules,

    cyclohexane or chloroform are such solvents. They have no hydrogen bonding and are

    Theory

    Color I2solution +

    H2SO4 + Starch

    Color at end

    Point

    Color I2solution +

    H2SO4 + Starch

    Color at end

    Point

    Our Experiment

  • Fractional Distillation Page 12

    only very slightly polar. Energywise, it is more favorable for the iodine to dissolve in the

    non-polar solvent than in the water, so it exists preferentially (but not totally, an

    equilibrium will exist) in the non-polar solvent. The release of energy as the iodine

    switches solvents is partially responsible for the initial build up of pressure in the

    separatory funnel, so two layers are produced when the two solvents are added together.

    In short Iodine, is slightly soluble in aqueous solutions, is more soluble in

    dichloromethane. Therefore, when aqueous solution containing iodine is placed in contact

    with dichloromethane, the iodine migrates into (is extracted by) the dichloromethane

    layer. The first step that done is take 10 mL of I2 solution 0,1 M brownish orange .Then

    diluted with aquadest on volumetric flask 100 mL . After diluted , take solution of the

    results of dilution with using volumetric pipette 10 mL and poured into separating funnel.

    The reaction occur is

    I2(aq) + H2O(l) no reaction occur

    After that added chloroform solution 5 mL as an organic solvent and shake 2-5

    times until two layer separated perfectly. That was obtained two layers, upper layer is

    water layer brownish orange and bottom layer is organic layer purple. The reaction that

    occur is

    3I2(aq) + 2CHCl3(aq) 2CHCl3(aq) + 3Cl2(g)

    After that separate organic layer with take out into beaker glass, it do repeatedly

    until all the organic layer are strictly separated entirely. Based on the theory, when

    aqueous solution containing iodine is placed in contact with dichloromethane, the iodine

    migrates into (is extracted by) the dichloromethane layer. Iodine in an aqueous solution

    appears brown. From theory we know that the color is shown in the picture below (left

    picture) and our experiment (right picture). We can assume that based on the theory our

    result is right

  • Fractional Distillation Page 13

    The water layer moved into erlenmeyer .After moved into erlenmeyer added 2 mL

    H2SO4 2M. The role of H2SO4 added is because in iodometric titrations are carried out in

    strongly acid media, a situation that promotes the reaction between oxidizing agents and

    iodide, and also H2SO4 is a strong acid and will deliver H+ which will help to proceed the

    reaction much faster or as a catalyst. And then added 1 mL starch solution 2 % that make

    changing color to blackish blue. Starch solution is added as an indicators for titration,

    when starch is mixed with iodine in water, an intensely colored starch/iodine complex is

    formed. Many of the details of the reaction are still unknown. The iodine/starch complex

    has energy level spacings that are just so for absorbing visible light- giving the complex

    its intense blue color. The complex is very useful for indicating redox titrations, when

    there is excess oxidizing agent, the complex is blue; when there is excess reducing agent,

    the I5-

    breaks up into iodine and iodide and the color disappears. Titrate solution using

    Na2S2O3 0,01M. The reaction that occur is

    I2 + 2e- 2I-

    2 S2O3 2-

    S4O62-

    + 2e-

    I2 + 2 S2O3 2-

    2I- + S4O6 2-

    Extraction iodine do 3 times, which also continue with the titration repeated 3

    times to get valid results. Based on the theory, the end point of I2 is changing color

    Color of layer that

    already wholly

    separated

    Theory

    Color of layer

    when Iodine

    extracted with

    Color of layer that

    already wholly

    separated

    Color of layer

    when Iodine

    extracted with

    Our Experiment

  • Fractional Distillation Page 14

    became colorless. From theory we know that the color is shown in the picture below (left

    picture) and our experiment (right picture). We can assume that based on the theory our

    end point is right.

    In first titration, volume of Na2S2O3 needed when solution change from purpleish

    black to colorless is 3,7 mL. With known volume of Na2S2O3 in titrations, we can

    calculate coefficient distribution iodine, the calculation below:

    Theory

    Color

    I2solution +

    H2SO4 +

    Color at end

    Point

    Color

    I2solution +

    H2SO4 +

    Color at end

    Point

    Our Experiment First

    Color

    I2solution +

    H2SO4 +

    Color at end

    Point

    Our Experiment Second Titration

    Color

    I2solution +

    H2SO4 +

    Color at end

    Point

    Our Experiment Third

  • Fractional Distillation Page 15

    ( )

    ( ) ( )

    ( )

    ( )

    [ ]( )

    [ ]( )

    [ ]( )

    [ ]( )

    Coefficient distribution (KD) iodine in first titration based on the calculation is

    2,86.

    In second titration, volume of Na2S2O3 needed when solution change from

    purpleish black to colorless is 3,8 mL. With known volume of Na2S2O3 in titrations, we

    can calculate coefficient distribution iodine, the calculation below:

    ( )

    ( ) ( )

    ( )

    ( )

    [ ]( )

    [ ]( )

    [ ]( )

    [ ]( )

    Coefficient distribution (KD) iodine in second titration based on the calculation is

    3.

    In third titration, volume of Na2S2O3 needed when solution change from purpleish

    black to colorless is 3,5 mL. With known volume of Na2S2O3 in titrations, we can

    calculate coefficient distribution iodine, the calculation below:

  • Fractional Distillation Page 16

    ( )

    ( ) ( )

    ( )

    ( )

    [ ]( )

    [ ]( )

    [ ]( )

    [ ]( )

    Coefficient distribution (KD) iodine in third titration based on the calculation is 3,14.

    Based on the calculation that have been gained above the value of KD on each titration

    the value of KD iodine average is 3.

    X. DISCUSSION

    From the results that we obtained, the value of coefficient distribution of iodine equal

    to 3 it is deviated from the theory. While value of coefficient distribution of iodine from

    theory is 10. This may due to some of the errors or mistakes have been occurred during the

    experiment. First and foremost is, iodine solution that we use in experiment is maybe has

    contaminant so it can affect the end point of titration, so the volume of Na2S2O3 that needed

    for determine mole of I2 is decrease and make whole calculation to determine coefficient

    distribution of iodine became not closely to coefficient distribution of iodine in theory.

    Second, is mistake occur when we do the titration, the reading of meniscus in burrette that

    contain Na2S2O3 that needed to achieve end point in titration is deviated, so the volume that

    needed may not be accurate. Beside it, human error may occur when measure the volume of

    materials that used in experiment, so the volume that needed may not be accurate and all this

    careless mistake may contribute to the inaccuracy of the result of value of coefficient

    distribution of iodine.

  • Fractional Distillation Page 17

    XI. CONCLUSION

    From this experiment we conclude that; first Iodine can extract in organic

    solvent, namely chloroform, that proven by two layer of organic layer(bottom) and

    water layer (upper)that formed. Second, the coefficient distribution (KD) Iodine is 3.

    XII. QUESTION AND ANSWER

    A. Question

    1. What is the difference between KD and D ?

    2. What if value of KD is same with D?

    3. How to find the value of the relationship between KD and D for a

    weak acid HB ? A weak acid HB that experienced dimerization in an organic

    solvents ?

    4. How to find the value of the relationship between KD and D for a

    weak base that ionize in water solvent and not react in organic solvent?

    5. Prove that with multiple extraction will have increases percent result,

    than just one extraction?

    Answer

    1. KD is the distribution coefficient or partition coefficient a special type

    of equilibrium constant which is related to the relative solubilities of the solute

    in the two solvents. Often one solvent is water and the other is an organic

    solvent. D is the distribution ratio, Distribution ratio(D) to account for the total

    concentration of species in two phases.

    The difference between D and KD is we use D when we calculate the total

    concentration of solute on organic solvent and water solvent, but in KD we just

    use the ratio concentration of solute into organic solvent and water solvent.

    2. Its mean that the only reaction affecting extraction efficiency is the

    solutes partitioning between the two phases.

    We can assume that the solute is initially present in the aqueous phase and that

    we are extracting it into the organic phase. A conservation of mass requires

    that the moles of solute initially present in the aqueous phase equal the

  • Fractional Distillation Page 18

    combined moles of solute in the aqueous phase and the organic phase after the

    extraction.

    3. The equilibrium reactions affecting the extraction of the weak acid,

    HA, by an organic phase in which ionic species are not soluble. In this case

    the partition coefficient and the distribution ratio are

    Although the weak acid is soluble in both phases, its conjugate weak base, A,

    is soluble only in the aqueous phase. The Ka reaction, which is called a

    secondary equilibrium reaction, affects the extraction efficiency because it

    controls the relative abundance of HA in solution.

    4. Because the weak base exists in two forms, only one of which extracts

    into the organic phase, the partition coefficient, KD, and the distribution ratio,

    D, are not identical.

    Using the Kb expression for the weak base,

    For the concentration of HB+ and substitute back into the equation for D,

    obtaining

  • Fractional Distillation Page 19

    5. Multiple extraction is always more efficient than simple one simple

    extraction, as explained when a solute is being extracted from an aqueous

    phase using an organic solvent, a better recovery will be obtained by using two

    equal volumes of solvent than the recovery that would be obtained using all

    the solvent in one large volume. This is all related to partition coefficients.

    The solubility of a material in two phases. If the material has a partition

    coefficient lets say of 4:1 . A single extraction will yield a ratio of 4:1,

    however if you do multiple extractions with a lower volume, each one will

    yield 4:1. So in total you will achieve a greater yield with multiple extractions,

    using smaller quantities.

  • Fractional Distillation Page 20

    REFERENCES

    Franek, Joseph.2000. Extractions.(online)

    (https://www.chem.umn.edu/services/lecturedemo/info/Extraction.html ) (access in

    13/5/2015 1:55AM)

    Harper college tutor.(noyear). Separatory Funnel. (online)

    (http://www.harpercollege.edu/tm-

    ps/chm/100/dgodambe/thedisk/labtech/sepfun2.htm ) (access in 13/5/2015 2:10 AM)

    Harvey ,L David.2011. LiquidLiquid Extractions.(online)

    (http://chemwiki.ucdavis.edu/Analytical_Chemistry/Analytical_Chemistry_2.0/07%3

    A_Collecting_and_Preparing_Samples/7G%3A_LiquidLiquid_Extractions ) (access

    in 13/5/2015 1:50AM)

    Matthew. 2011. Extraction and Determination of a Distribution Coefficient

    (Kd) . (online)

    (http://www.mendelset.com/articles/685/extraction_and_determination_distribution_c

    oefficient_kd ) (access in 13/5/2015 2:10 AM)

    Pahlavan. (noyear) . Determination of Distribution Coefficient. (online)

    (http://swc2.hccs.edu/pahlavan/2423L6.pdf ) (access in 13/5/2015 2:13 AM)

    TimPenyusun .2015. Panduan Praktikum Kimia Analitik II: DDPK. Surabaya:

    Jurusan Kimia FMIPA Unesa

    Underwood,A.L dan Day.R.A.Jr.2002. Analisis Kimia Kuantitatif Edisi

    Keenam. Jakarta: Erlangga

    Surabaya, May 18th

    , 2015

    Mengetahui,

    Dosen/Asisten/Pembimbing, Praktikan,

    (.) ()

  • Fractional Distillation Page 21

    ATTACHMENT

    Iodium solution 0,1M

    has yellowish brown

    color

    Making 100mL iodium

    solution, the color was

    yellowish brown

    Put the 10 mL of iodium

    solution into separated

    funnel

    Chloroform solution was

    colorless

    The solution formed two

    layers after added by

    chloroform

    Water Phase has

    orangish brown Color

    of solution

    Organic Phase has

    purple Color of

    solution

  • Fractional Distillation Page 22

    Shaking the solution to separate the

    organic phase and water phase

    Turn the tap to separate

    the organic phase

    The organic phase was

    purple solution

    The orangish brown

    water phase in separated

    funnel

    Shaking again to separated organic

    phase with water phase certainly

    Separated again The water phase that

    left in separated funnel

    Pouring to Erlenmeyer

    flask, repeat until 3 times

  • Fractional Distillation Page 23

    Water phase was adding

    with H2SO4

    Water phase was adding

    with Starch solution

    The color of solution

    become blackish purple

    Na2S2O3(aq) 0,01M,

    colorless solution

    Titrate with Na2S2O3(aq)

    0,01M

    Initial scale

    was 0 mL

    Final scale

    was 3,7 mL

    The solution after titrate

    become colorless solution

    Second water phase was

    added with H2SO4 too.

    And adding with Starch

    solution

  • Fractional Distillation Page 24

    Titrate with Na2S2O3(aq)

    0,01M

    The solution after titrate

    become colorless

    solution

    Initial scale

    was 5 mL

    Final scale

    was 8,8mL

    Initial scale

    was 9 mL

    Final scale was

    12,5 mL

    Third water phase was added

    with H2SO4 and Starch solution

    Titrate with Na2S2O3(aq)

    0,01M

    Three of Erlenmeyer which is after titrated

  • Fractional Distillation Page 25

    Iodium solution that added

    with H2SO4 and Starch

    solution

    The color of solution

    become blackish purple

    Titrate with Na2S2O3(aq)

    0,01M

    Initial scale was

    13 mL

    Final scale was 22

    mL

    The solution after titrate

    become colorless

    solution

  • Fractional Distillation Page 26

    CALCULATION

    Reaction :

    I2+ 2e - 2I- x 2

    2S2O32-

    S4O6+ 4e-

    x 1

    2I2 + 2S2O32-

    4I- + S4O6

    - Comparison solution / I2 standard

    N Na2S2O3 = 0,01 N

    V Na2S2O3 = 9 mL

    mmolek I2 = mmolek S2O32-

    mmolek I2 = VS2O32-

    x N S2O32-

    mmolek I2 = 9 mL x 0,01 N

    I2 = 0,09 mmolek x

    I2 standard = 0,045 mmol

    - First titration

    VNa2SO3 = 3,7 mL

    mmolek I2 = mmolek S2O3-

    mmolek I2 = V S2O3-x Na2SO3

    2-

    mmolek I2 = 3,7 mmolek x 0,01 N

    I2 = 3,7 mL x

    I2 (a ) = 0,0185 mmol

    Mmol I2(0) = mmol I2 standard mmol I2(a)

    = 0,045 0,0185

    = 0,0265 mmol

    [I2](a) =

    = 0,00185

    [I2](0) =

    = 0,0530

    KD = [ ]( )

    [ ]( )

  • Fractional Distillation Page 27

    - Second Titration

    VNa2SO3 = 3,8 mL

    mmolek I2 = mmolek S2O3-

    mmolek I2 = V S2O3-x Na2SO3

    2-

    mmolek I2 = 3,8 mL x 0,01 N

    = 3,8 mL x

    I2 (a ) = 0,0180 mmol

    Mmol I2(0) = mmol I2 standard mmol I2(a)

    = 0,045 0,0180

    = 0,027 mmol

    [I2](a) =

    = 0,00180

    [I2](0) =

    = 0,0054

    KD = [ ]( )

    [ ]( )

    - Third Titration

    VNa2SO3 = 3,5 mL

    mmolek I2 = mmolek S2O3-

    mmolek I2 = V S2O3-x Na2SO3

    2-

    mmolek I2 = 3,5 mmolek x 0,01 N

    I2 = 0,035 mmolek x

    I2 (a ) = 0,0175 mmol

    Mmol I2(0) = mmol I2 standard mmol I2(a)

    = 0,045 0,0175

    = 0,0275 mmol

    [I2](a) =

    = 0,00175

    [I2](0) =

    = 0,0055

    KD = [ ]( )

    [ ]( )

    KD average =

    = 3