Making of Standardization Solution KMnO4, And Determine of Mixture Fe2+ and Fe3+

Sri Agustiani Basir Department of Chemistry, Makassar State University

Abstract Permanganometri titration is carried out based on the reaction by potassium permanganate (KMnO4). This reaction is focused on the oxidation and reduction reactions that occur between KMnO4 with certain raw materials. The purpose of the experiment Determination of Fe with Permanganometri way is to determine the levels of iron (Fe) contained in the sample. Materials used in these experiments were samples containing Fe, potassium permanganate (KMnO4) sulfuric acid (H2SO4) and oxalic acid (H2C2O4). While the tool used is a set of standardized tools, heaters, measuring cups, and pipette volume erlenmeyer. This experimental procedure is the preparation of a solution of potassium permanganate and potassium standardization permaganat by titrating the solution using sulfuric acid and determine the iron content by titrating the samples using a solution of potassium permanganate. From these experiments show that the levels of ferro and ferri in the sample 4.28 mg/mL and 0.51 mg mL. Key words: Permanganometri, Titration, KMnO4

1. Introduction Titration, also known as titrimetry, is a common laboratory method of quantitative chemical analysis that is used to determine the unknown concentration of an identified analyte. Because volume measurements play a key role in titration, it is also known as volumetric analysis. A reagent, called the titrant or titrator is prepared as a standard solution. A known concentration and volume of titrant reacts with a solution of analyte or titrand to determine concentration (Anonyma. 2011).

Permanganometry is one of the techniques used in qualitative analysis in Chemistry. It is a redox titration and involves the use of permanganates and is used to estimate the amount of analyte present in unknown chemical samples. It involves two steps, namely the titration of the analyte with potassium permanganate solution and then the standardization of potassium permanganate solution with standard sodium oxalate solution. The titration involves volumetric manipulations to prepare the analyte solutions (Anonymb. 2011). Permanganometri is a titration is based on redox reactions. In this reaction, ion of MnO4- acts as an oxidant. MnO4- ion will be changed to Mn2+ ions in acidic conditions. Titration technique is commonly used to determine the levels of oxalate or iron in a sample. Potassium permanganate is an oxidant that is best for determining the levels of iron contained in the sample under acidic conditions using a solution of sulfuric acid (H2SO4) (Khopkar. 2008:53) The aim of experiment are to know making of standard solution of KMnO4, to know the standardization solution and calculate the normality of KMnO4 standard solution and to know the determine mixture of ferro and ferri.

2. Experiment 1. Preparation of standard solution KMnO4 Preparation of standard solution KMnO4 by dissolving crystals KMnO4 with aquadest. To weight 1.6 gram of KMnO4 with watch glass. To put into a

beaker glass 1000 mL, to add 500 mL aquadest and then to close a beaker glass with watch glass. To boil the KMnO4 solution until 30 minutes, and then cooled. 2. Standardization solution Standard solution is a chemical term that indicates that a solution of known concentration. Standardization is the process of developing and implementing technical standards. To weight 0.65 gram crystal oxalate acid and to dissolve with

aquades and to dilute to become 100 mL. To take 25 mL solution and then

to add 5 mL H2SO4 and to heat until

70o C. In hot conditions, solution

titrated with standard KMnO4 until purple colors of permanganate solution droplets are not lost. To repeat titration until 3 times and to note the average of volume titration. To calculate the normality of standard solution KMnO4. 3. Determine of mixture ferro and ferri To dropper 25 mL mixture of sample solution, to add 25 mL H2SO4 1 N solution. Titrate a solution with KMnO4 of standard solution until become young purple (1-2 drops of color from the excess KMnO4 solution). To note the average of titrant volume. To put 25 mL sample solution, to add 10 mL of concentrated HCl and to heat until 70oC. In hot conditions, to add a few drops SnCl2 5% solution until the yellow color disappeared and turned into green. Cooled the solution and then to add 10 mL HgCl2 5% to form while precipitate HgCl2. Titrated solution with KMnO4 standard until to form purple solution. To note the volume of titrant. To repeat titration until 3 times and note the average of volume titrant. To calculate the content of ferro and ferri in mixture.

4. Result and Discussion 1. Preparation of standard solution KMnO4 1.6 gram KMnO4 + 500 mL aquades purple solution purple solution purple solution (standard solution). Standard solution is a solution of known concentration, which will be used in volumetric analysis. Preparation of KMnO4 standard solution by dissolving crystals of KMnO4 with aquades. KMnO4 solution was heated to give a solution purple. KMnO4 solution then cooled and put in a brown bottle because KMnO4 is a strong oxidizer so it is very easy to react when exposed to sunlight.

2. Standardization of KMnO4 a. 0.6 gr oxalate acid oxalate acid b. 25 mL oxalate acid + 5 mL concentrated H2SO4 70oC colorless solution faint purple solution. colorless solution 100 mL solution of

Volume of titrant Volume of titrant (mL) Data Analysis : Known : V1 V2 W : 21 mL : 20.4 mL : 0.65 gr = 650 mg I 21 II 20.4

BM C2H2O4 : 126 mg/mmol Asked : Normality of KMnO4 Resolving Vaverage KMnO4 :

:
: 20.7 mL

N KMnO4

: : 0.12 mmol/mL = 0.12 N Titration is the process of measuring the volume of solution contained in the burette is added into another solution of known volume until there is complete reaction. Solution of known concentration is called the standard solution. The process of determining the concentration of the standard solution is called standardization. Standard solution that is two standard

solutions of primary and secondary standard solution. Secondary standard solution is a solution whose concentration is obtained by titrating with a solution of primary standard, usually through titrimetry. KMnO4 solution is a secondary solution, therefore standardized KMnO4 solution with a solution of oxalic acid as the primary standard solution. solution of oxalic acid is the solution to be titrated was added concentrated sulfuric acid which serves to provide acidic conditions. KMnO4 is a strong oxidizing nature auto indicator and also because it changes color from clear colorless to purple. So the observed endpoint titration is easier. To standardize the KMnO4 solution made warming of the oxalic acid solution was added concentrated sulfuric acid until the reaction temperature of 700 C in order to run fast. Average volume of 20.7 mL obtained in order to obtain the normality of 0.12 N. Reactions that occur in the standardization of KMnO4 with oxalic acid solution: 2 KMnO4 + 5 H2C2O4 + 3 H2SO4 2 MnSO4 + 10 CO2 + 8 H2O + K2SO4 3. Determine of mixture ferro and ferri a. 25 mL of sample solution (faint yellow) + 25 mL of H2SO4 more faint yellow purple solution

Volume of titrant Volume of titrant (mL) I 13.7 II 16.5

b. 25 mL of sample solution (faint yellow) + 10 mL HCl yellow solution 700C + SnCl2 greenish yellow + 10 mL HgCl2

brownish yellow Volume of titrant Volume of titrant (mL) Data Analysis : Known : Va1 : 13.7 mL I 16.9 II 16.9

Va2

: 16.5 mL

Vb1 : 16.9 mL Vb2 : 16.9 mL N KMnO4 : 0.12 N BM Fe : 59 mg/mmol Asked : Content of ferro and ferri

Resolving

= 4.28 mg/mL

= = = 0.51 mg/mL a. Determine of ferro In this experiment used the sample solution and the mixture ferri and ferro and add H2SO4 that function to acidify the iron to

soluble iron, and then titrated with KMnO4 produces a purple solution. In the process of Fe2+ ion titration will be oxidized by MnO4- of titrant Fe3+ ions formed by the reaction: MnO4- + 8 H+ + 5 Fe 2+ Mn2+ + 5 Fe3+ + H2O

Titration end point can be seen from the color change of yellow to a purple solution. From the results obtained by titration of the average volume of 15.1 mL with ferro content in the sample solution of 4,28 mg/mL. b. Determine of ferri In this experiment used a solution of ferro and ferri sample mixture, then add HCl that serves to accelerate the reaction between the sample solution and HCl. The solution add SnCl2 5% to help the dissolving process and to reduce the iron ions Fe3+ to Fe2+. This addition causes the color change from yellow to green Fe3+. The reaction is: Sn2+ + 2 Fe3+ Sn4+ + 2 Fe2+ But, in this experiment the color of the solution does not fit with the theory that is green but the greenish yellow color. This happens because all the Fe3+ ions are not completely reduced to Fe2+ ions due to the lack of addition of SnCl2 solution in the solution. After it was added HgCl2 no white precipitate formed in the absence of excess Sn2+ ions in solution. The solution is titrated to brownish green. Titration was repeated twice to obtain an accurate value. Average volume obtained and the levels of Ferri 16.9 mL in the sample solution was 0,51 mg / mL. His reaction: KMnO4 + 4 H2O + 2 FeSO4 MnSO4 + 4 H2O

5. Conclusion Conclusions of the research results obtained: 1. To make the standard solution of KMnO4 can done by diluting and heating 2. Normality which get from KMnO4 in this experiment is 0.12 N 3. The content of ferro is 4.28 mg/mL and ferri is 0.51 mg/mL

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2011. http://en.wikipedia.org/wiki/Permanganometry. November.

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Khopkar. 2008. Konsep Dasar Kimia Analitik. Jakarta: Universitas Indonesia