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CHEMISTRY 3B:SEC 5

Laboratory Report
Synthesis And Analysis Of Potassium Ferric Oxalate
Akwasi Dekyi Jr. 11/27/2009

Dr. Vandana A. Bindra

Introduction
This experiment involves the synthesis (combination of entities) of potassium ferric oxalate and the verification of the purity and the composition of the product derived. In this series of experiment potassium ferric oxalate will be made and analyzed. It will be analyzed in two ways. The amount of potassium ferric oxalate will be determined using a titration method. After that an independent analysis will be done by using a spectrophotometer to determine the concentration of iron in the sample. The equation for the overall reaction to obtain potassium ferric oxalate is as follows: 2FeC2O4.2H2O(s) + H2O2(aq) +H2C2O4(aq) + 3K2C2O4(aq) 2K3Fe(C2O4)3.3H2O(s) In order for potassium ferric oxalate to be produced, ferrous oxalate must be formed. The equation for the formation of ferrous oxalate is given as follows: Fe(NH4)2.SO4.6H2O(aq) + H2C2O4(aq) FeC2O4.2H2O(s) + 2(NH4)HSO4(aq).3H2O(s) Before we determined the concentration of iron in our sample, the iron in our product was made into a new complex using phenanthroline molecule. Then iron was reduced by the compound hydroxylamine hydrochloride. The equation for the formation of the complex iron (ii) and the reduction of iron (iii) by hydroxylamine is as follows: Fe+2 + 3C12H8N2 Fe(C12H8N2)3+2 (Formation of Fe+2) 4Fe+3 + 2H2NOH 4Fe+2 + N2O + 4H+ + H2O (Reduction of Fe+3) The amount of oxalate ion in the sample was then determined by titrating the solution of the product with potassium permanganate. The equation is given as follows; 5C2O4-2 + 2MnO4- + 16H+ 10CO2 + 2Mn+2 + 8H2O

Method
The instruments used for this experiment were; beakers to contain the samples, Bunsen burner for the conversion of compounds, a spectrophotometer to read the absorbance and transmittance of complex solutions, filter paper for the separation of the solid from the aqueous solution, burette for titration, thermometer for temperature readings, pipette for transferring the liquid, volumetric flasks and test tubes . The synthesis of the co-ordination compound, potassium ferric oxalate trihydrate was done by firstly by the preparing ferric oxalate. This was done by adding a sufficient amount of Fe (NH4)2(SO4)2.6H2O with H2SO4 and oxalic acid which in this experiment was 5grams. The solution

was clamped to a ring stand and using a Bunsen burner the solution was heated to allow the reaction to occur. A yellow solid then appeared when the reaction occurred, this solid was FeC2O4.2H2O. The yellow liquid was then poured and the flask was again placed on the ring stand and 20ml of deionized water was added to the solid and was heated again. The solution was heated again get rid of the ammonium bisulfate tetra hydrate (2(NH4)HSO4 + 4H2O).This was then mixed with deionized water and after it settled was decanted (Separated solid from the aqueous solution). 10 ml of saturated Potassium oxalate was then added to the solid. A solution of 20ml of 3% H2O2 was made a place in a beaker and 8ml of 1M of H2C2O4 was also made and placed into a graduated cylinder. The solid was then heated to 40:C so that the product will not be lost as a result of overheating.20 ml of H2O2 was added slowly (used a transfer pipette) to allow the full reaction to occur. When substances are added slowly to other compounds during a chemical reaction, it reduces the chances of having side reactions and also allows the full reaction to occur. The solution was then heated to boil and then the 5ml of 1M of H2C2O4 was then added all at once. The solution was then filtered using a filter paper in its heated state to allow the yellow solid to separate completely from the aqueous solution. Ethyl alcohol was added to the solution to kick off the formation of the crystals. The solution was left for a week to allow some of the liquid to evaporate and the crystals to grow. The quality and quantity of crystals formed depended significantly on the accuracy and purity of the procedure/experiment carried out. The crystals were then collected a week after and were rinsed with deionized water and alcohol. They were then blotted dry so that the solution going to be made for the analysis of iron in the compound will not be contaminated. Two solutions were made using the sample of crystals. The solution we called A was made by adding 20ml of 3M H2SO4 and 50ml of deionized water to 1.00gram sample of the crystals. The second solution, we called B, was nothing less than a diluted version of the solution A. 5ml of A was added to 100ml of deionized water to form solution B. Then 5ml of solution B was added to 10ml of 1M of sodium acetate and 2ml of 10% hydroxylamine hydrochloride. 3ml of .25% of C12H8N2 was then added and mixed all in a volumetric flask. Solution was then diluted with deionized water till it reached the 100ml mark on the flask. A spectrometric analysis was then done to help is determine the concentration of iron in the solution. We set the spectrophotometer to 508 nm because the absorption spectrum of ferrous phenalthroline has a peak at 508nm and read each of the absorbance and transmittance of the complex solutions. We used the absorbance and concentration of standard complex solutions read using a spectrophotometer, to calibrate a curve to determine the concentration of the solution. As a side remark I tried to use beer law to derive the concentration of the solution but was

ineffective due to the fact that there was no known absorptivity and path length. The analysis of oxalate in the compound was done in an oxidation reduction titration. The most important but of this procedure to was transfer electrons from one species to another. A derived amount of Potassium permanganate was titrated against a known volume of standard oxalic acid. With my calculations I had 0.05L/50ml of permanganate diluted with about 200ml of deionized water titrating against 1.58grams of oxalic acid diluted with 100ml of deionized water.20ml of oxalic acid solution was added to 10ml of deionized water and 15ml of 3M of sulfuric acid and was heated to 80C. It was then titrated with potassium permanganate in its heated state until the solution showed pink. The volume was then recorded. We did that about two times. In determining the percent of oxalate in the compound the same procedure was taken as with the oxalic acid. Instead in the oxalic acid we used 20ml of sample A and titrated it also in its heated state with potassium permanganate. The volume at which the sample turned picked was also recorded.

Results: Quantitative Data Derived


Table 1:Analysis Of Fe(NH 4 ) 2 (SO 4 ) 2 .6H 2 O
Weight Of Fe(NH4)2(SO4)2.6H2O Moles Of Fe(NH4)2(SO4)2.6H20 Theoretical Yield Actual Yield Percent Yield 5.00grams 0.128 moles 6.26grams 1.91grams 30.51%

Table 2: Calibration Curve data


[Fe+2)[M] Transmittance Absorbance Standard 2.00E-05 55.1 0.34 1 Standard 4.00E-05 30.1 0.52 2 Standard 6.00E-05 17.9 0.75 3 Standard 8.00E-05 9.9 1.09 4 Solution 7.22E-05 11.2 0.95 C

Graph1:Calibrated Curve

Spectrophotometric Analysis Of Iron Content


1.2 1 0.8 0.6 0.4 0.2 0 0.00E+00 2.00E-05 4.00E-05 y = 12400x + 0.055 Absorbance

6.00E-05

8.00E-05

1.00E-04

Conentration(Fe+2)[M]

Table 3: Analysis of iron in K 3 Fe(C 2 O 4 ) 3 .3H 2 O


Weight of K3Fe(C2O4)3.3H2O used in solution A Moles Of Fe3+ in Solution A(mol) Weight Of Fe3+ Solution A(grams) Actual Weight % Of Fe3+ in K3Fe(C2O4)3.3H2O Theoretical weight percent of Fe3+ in K3Fe(C2O4)3.3H2O Percent Error in % Of Fe3+ 1.00grams 0.00289moles 0.161grams 16.1% 11.4% 29.2%

Table 4: Standardization of KMnO 4 solution


Weight Of H2C2O4.2H2O(g) Molarity Of H2C2O4.2H2O solution(M) 1.58 grams 0.05M

Volume Of H2C2O4.2H2O solution(mL) Moles Of oxalate (mol) Initial buret reading (mL) Final buret reading (mL) Volume of KMnO4(mL) Moles Of KMnO4(mol) Molarity Of KMnO4 solution (M)

Run #1 20 ml 0.001 moles 1.3 ml 21.4 ml 20.1 ml 0.0004 moles 0.0190

Run #2 20ml 0.001 moles 0.1ml 20.3 ml 20.2 ml 0.0004 moles 0.0198

Average Molarity of KMnO4 solution (M) 0.0194 (M)

Table 5: Titration of solution A


Volume of solution A Initial buret reading(mL) Final buret reading(mL) Volume of KMnO4 solution Moles of KMnO4(mol) Moles&Molarity of oxalate(mol) Run #1 20 ml 10.02ml 33.78ml 23.58 ml Run #2 20 ml 0.10ml 23.31ml 23.41 ml

4.57e-4 moles 4.57e-4 moles 1.14e-3moles&0.057(M) 1.14e-3moles &0.056(M)

Average Moles/Molarity of oxalate (mol) 1.14e-3moles&0.0565(M)

Table 6: Analysis of oxalate in K 3 Fe(C 2 O 4 ) 3 .3H 2 O


Average moles of oxalate Total moles of oxalate in solution A Total weight of oxalate(g) Wt of K3Fe(C2O4)3.3H2O used to make solution A(g) Actual weight percent oxalate in K3Fe(C2O4)3.3H2O Theoretical weight percent oxalate in K3Fe(C2O4)3.3H2O Percent error in percentage oxalate 1.14e-2moles 5.65e-3 moles 0.498grams 1.00gram 49.8% 53.8% 8.03%

Table 7: Analysis of ration between the moles of oxalate to Fe in crystals


Moles of oxalate in 1g of the K3Fe(C2O4)3 Moles of Fe+3 in 1g of the K3Fe(C2O4)3 Ratio: Moles oxalate/Moles Fe+3 % Comparison with the theoretical ratio 1.14e-3moles(0.00114moles) 0.00289 moles 0.00114: 0.00289-1:2.5

Conclusion & Discussion


Overall this was a successful experiment. However there were some limitations during the experiment that affected my results. I will start with the production of Fe(NH4)2(SO4)2.6H2O. My actual yield of crystals was 1.92grams as opposed to the theoretical yield which was 6.26grams.This brought my percent yield down to 30.51% which to me was relatively low. This may have been caused during the preparation of my crystals. Some of my solid may have been lost during the heating process in the course of allowing the reaction to occur. The concentration of solution C which I derived from calibrating a curve with the known absorbance and concentrations of the complex solution helped me determine the concentration of solution A. Solution A was nothing more than a dilution of solution C. The equation derived for the relationship of solution C to solution A was [M]solution A (Molarity of solution A) =400*[M] of solution C. In any event this helped me determine the moles of oxalate I had present in the solution A for the analysis of iron. The weight of iron I derived was relatively low as compared to the theoretical weight of iron. This may have been caused during the course of my experiments. I didnt fully allow my products (green crystals) to dry out completely before I prepared the solution which may have most likely contaminated my solution affecting the concentration of iron in the solution which then affected the amount of iron in the solution. I feel if I had left my crystals to dry out well, the weight of iron in the solution would have been more. The ratio of

Calculations
Moles Of Fe(NH4)2(SO4)2.6H20= 5.00grams Of Fe *1mole Fe/391.8grams of Fe=0.0128moles Theoretical yield= 491KFO/392FNS=Xgrams/5.00g FNS=6.36grams of Potassium iron(iii)oxalate Actual yield=Derived from experiment (1.91grams) Percent Yeild=1.91grams/6.26grams *100=30.51% Concentration of A= Y=12400x +0.055Y=0.95X=7.22E-5 7.22E-5 x 400=0.0289(M) Moles Of Fe+3=0.0289 x 0.1(100ml)=0.00289moles

Wt of Fe3+(grams)=0.00289moles x 55.847(molar mass of Fe)=0.0161grams Actual Wt % of Fe3+ in K3Fe(C2O4)3.3H2O=0.161g/1.0g x 100%=16.1% Theoretical Weight of Fe3+ in K3Fe(C2O4)3.3H2O=55.85(Wt Fe)/491.2(Wt of compound)=11.47% Percentage Error=11.47-16.1/16.1 x 100=29.2% Weight Of H2C2O4.2H2O=>X/0.250L=0.050.0125moles of H... x 126.07g(wt of H..)=1.58g Molarity of H2C2O4.2H2O solution=0.05(M) Volume of H2C2O4.2H2O=20ml(0.02L) Moles of oxalate=Molarity of oxalic acid(0.05[M]) x the volume oxalic acid(0.020)=0.001moles Moles of KMnO4= 0.001moles x 2/5= 0.004moles Molarity of KMnO =0.004moles/0.0201 & 0.004/0.0201=

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