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

Dr. Vandana A. Bindra

Then iron was reduced by the compound hydroxylamine hydrochloride. It will be analyzed in two ways. 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. pipette for transferring the liquid. Bunsen burner for the conversion of compounds. burette for titration. The equation for the overall reaction to obtain potassium ferric oxalate is as follows: 2FeC2O4.3H2O(s) Before we determined the concentration of iron in our sample. volumetric flasks and test tubes . The equation for the formation of ferrous oxalate is given as follows: Fe(NH4)2.SO4.2H2O(s) + 2(NH4)HSO4(aq). The equation is given as follows. ferrous oxalate must be formed. beakers to contain the samples.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.6H2O with H2SO4 and oxalic acid which in this experiment was 5grams. In this series of experiment potassium ferric oxalate will be made and analyzed. the iron in our product was made into a new complex using phenanthroline molecule. This was done by adding a sufficient amount of Fe (NH4)2(SO4)2.2H2O(s) + H2O2(aq) +H2C2O4(aq) + 3K2C2O4(aq) 2K3Fe(C2O4)3. The solution . filter paper for the separation of the solid from the aqueous solution. potassium ferric oxalate trihydrate was done by firstly by the preparing ferric oxalate.3H2O(s) In order for potassium ferric oxalate to be produced. 5C2O4-2 + 2MnO4. 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. thermometer for temperature readings.6H2O(aq) + H2C2O4(aq) FeC2O4.+ 16H+  10CO2 + 2Mn+2 + 8H2O Method The instruments used for this experiment were. a spectrophotometer to read the absorbance and transmittance of complex solutions. The synthesis of the co-ordination compound.

it reduces the chances of having side reactions and also allows the full reaction to occur. 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. we called “B”.This was then mixed with deionized water and after it settled was decanted (Separated solid from the aqueous solution). As a side remark I tried to use beer law to derive the concentration of the solution but was . this solid was FeC2O4. The solid was then heated to 40:C so that the product will not be lost as a result of overheating. The solution was left for a week to allow some of the liquid to evaporate and the crystals to grow. Ethyl alcohol was added to the solution to kick off the formation of the crystals. 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. A spectrometric analysis was then done to help is determine the concentration of iron in the solution. 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. 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.25% of C12H8N2 was then added and mixed all in a volumetric flask. 10 ml of saturated Potassium oxalate was then added to the solid. The solution was then heated to boil and then the 5ml of 1M of H2C2O4 was then added all at once.was clamped to a ring stand and using a Bunsen burner the solution was heated to allow the reaction to occur. 5ml of “A” was added to 100ml of deionized water to form solution B.20 ml of H2O2 was added slowly (used a transfer pipette) to allow the full reaction to occur. The solution was heated again get rid of the ammonium bisulfate tetra hydrate (2(NH4)HSO4 + 4H2O). When substances are added slowly to other compounds during a chemical reaction. Two solutions were made using the sample of crystals. 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.00gram sample of the crystals. to calibrate a curve to determine the concentration of the solution. 3ml of .2H2O. We used the absorbance and concentration of standard complex solutions read using a spectrophotometer. The solution we called “A” was made by adding 20ml of 3M H2SO4 and 50ml of deionized water to 1. Solution was then diluted with deionized water till it reached the 100ml mark on the flask. The second solution. was nothing less than a diluted version of the solution “A”. A yellow solid then appeared when the reaction occurred. Then 5ml of solution “B” was added to 10ml of 1M of sodium acetate and 2ml of 10% hydroxylamine hydrochloride.

The volume at which the sample turned picked was also recorded.9 1.6H 2 O Weight Of Fe(NH4)2(SO4)2. The volume was then recorded.34 1 Standard 4.00E-05 30.ineffective due to the fact that there was no known absorptivity and path length.52 2 Standard 6.00E-05 55.91grams 30. In determining the percent of oxalate in the compound the same procedure was taken as with the oxalic acid.2 0.00E-05 17.00grams 0.9 0.26grams 1.1 0.00E-05 9.09 4 Solution 7. We did that about two times.20ml of oxalic acid solution was added to 10ml of deionized water and 15ml of 3M of sulfuric acid and was heated to 80C.51% Table 2: Calibration Curve data [Fe+2)[M] Transmittance Absorbance Standard 2.05L/50ml of permanganate diluted with about 200ml of deionized water titrating against 1. A derived amount of Potassium permanganate was titrated against a known volume of standard oxalic acid.22E-05 11. Instead in the oxalic acid we used 20ml of sample “A” and titrated it also in its heated state with potassium permanganate. With my calculations I had 0. The analysis of oxalate in the compound was done in an oxidation reduction titration.6H2O Moles Of Fe(NH4)2(SO4)2.58grams of oxalic acid diluted with 100ml of deionized water.95 C .128 moles 6. Results: Quantitative Data Derived Table 1:Analysis Of Fe(NH 4 ) 2 (SO 4 ) 2 .1 0.6H20 Theoretical Yield Actual Yield Percent Yield 5.75 3 Standard 8. It was then titrated with potassium permanganate in its heated state until the solution showed pink. The most important but of this procedure to was transfer electrons from one species to another.

3H 2 O Weight of K3Fe(C2O4)3.00E-05 8.8 0.00E+00 2.00E-04 Conentration(Fe+2)[M] Table 3: Analysis of iron in K 3 Fe(C 2 O 4 ) 3 .Graph1:Calibrated Curve Spectrophotometric Analysis Of Iron Content 1.3 ml 21.055 Absorbance 6.2 1 0.0004 moles 0.4 ml 20.2 ml 0.00E-05 1.0190 Run #2 20ml 0.05M Volume Of H2C2O4.001 moles 0.0198 .3H2O Percent Error in % Of Fe3+ 1.1% 11.2H2O 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 0.1ml 20.00E-05 y = 12400x + 0.001 moles 1.3H2O Theoretical weight percent of Fe3+ in K3Fe(C2O4)3.0004 moles 0.2H2O solution(M) 1.6 0.2 0 0.00289moles 0.3H2O used in solution A Moles Of Fe3+ in Solution A(mol) Weight Of Fe3+ Solution A(grams) Actual Weight % Of Fe3+ in K3Fe(C2O4)3.58 grams 0.4% 29.2% Table 4: Standardization of KMnO 4 solution Weight Of H2C2O4.00E-05 4.3 ml 20.00grams 0.2H2O(g) Molarity Of H2C2O4.4 0.161grams 16.1 ml 0.

3H2O used to make solution A(g) Actual weight percent oxalate in K3Fe(C2O4)3.58 ml Run #2 20 ml 0.14e-3moles(0.00114moles) 0.14e-3moles&0.057(M) 1.02ml 33.5 .14e-2moles 5.10ml 23.0194 (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 10.0565(M) Table 6: Analysis of oxalate in K 3 Fe(C 2 O 4 ) 3 .3H2O Percent error in percentage oxalate 1.00114: 0.3H2O Theoretical weight percent oxalate in K3Fe(C2O4)3.31ml 23.14e-3moles &0.00gram 49.00289-1:2.03% 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 1.3H 2 O Average moles of oxalate Total moles of oxalate in solution A Total weight of oxalate(g) Wt of K3Fe(C2O4)3.57e-4 moles 1.41 ml 4.8% 53.14e-3moles&0.65e-3 moles 0.78ml 23.056(M) Average Moles/Molarity of oxalate (mol) 1.498grams 1.Average Molarity of KMnO4 solution (M) 0.8% 8.57e-4 moles 4.00289 moles 0.

The weight of iron I derived was relatively low as compared to the theoretical weight of iron.6H2O.92grams as opposed to the theoretical yield which was 6.This brought my percent yield down to 30. In any event this helped me determine the moles of oxalate I had present in the solution “A” for the analysis of iron. However there were some limitations during the experiment that affected my results. the weight of iron in the solution would have been more. 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”. I will start with the production of Fe(NH4)2(SO4)2. 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”. This may have been caused during the preparation of my crystals. This may have been caused during the course of my experiments.51% which to me was relatively low. Some of my solid may have been lost during the heating process in the course of allowing the reaction to occur. I didn’t 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.Conclusion & Discussion Overall this was a successful experiment. The ratio of . My actual yield of crystals was 1. Solution “A” was nothing more than a dilution of solution “C”.26grams.

0201 & 0.3H2O=0.6H20= 5.055Y=0. x 126.1 x 100=29.05(M) Volume of H2C2O4.847(molar mass of Fe)=0.47-16.05[M]) x the volume oxalic acid(0.8grams of Fe…=0.0289(M) Moles Of Fe+3=0.3H2O=55.2H2O solution=0.004moles/0.004moles Molarity of KMnO =0.00g FNS=6...00289moles x 55.58g Molarity of H2C2O4.07g(wt of H.0161grams Actual Wt % of Fe3+ in K3Fe(C2O4)3.2(Wt of compound)=11.001moles x 2/5= 0.00289moles            Wt of Fe3+(grams)=0.020)=0.91grams) Percent Yeild=1.004/0.0128moles Theoretical yield= 491KFO/392FNS=Xgrams/5.00grams Of Fe… *1mole Fe…/391.001moles Moles of KMnO4= 0.2% Weight Of H2C2O4.26grams *100=30.51% Concentration of A= Y=12400x +0.1(100ml)=0.1/16.)=1.02L) Moles of oxalate=Molarity of oxalic acid(0.91grams/6..95X=7.0201= .22E-5 7.Calculations      Moles Of Fe(NH4)2(SO4)2.0289 x 0.1% Theoretical Weight of Fe3+ in K3Fe(C2O4)3.22E-5 x 400=0.0g x 100%=16.250L=0.85(Wt Fe)/491.2H2O=20ml(0.0125moles of H.2H2O=>X/0.161g/1.47% Percentage Error=11.050.36grams of Potassium iron(iii)oxalate Actual yield=Derived from experiment (1.

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