In coordination chemical science there are different types of ligands. Monodentate ligands donate merely one lone brace to the metal ion. Bidentate ligands donate two braces of negatrons such as the oxalate ligands which can adhere at two sites with the metal ion, therefore a coordination figure of three ligands around one metal ion. Oxalate has four Os with each holding a lone brace but it merely uses two lone braces to organize a coordination compound. here are besides multidentate ligands such as the EDTA which donate more than two braces of negatrons. Oxalate is can be regarded as a chelating agent. This means that two or more bonds are being broken so that the ligand would be separated from the metal. These chelating ligands provide more stableness to the complex than those with monodentate ligands.
The K trioxalatoferrate ( III ) trihydrate and the Fe ( II ) oxalate have a stereochemistry of an octahedral. The oxalate ion is a weak field ligand harmonizing to the spectrochemical series. The Fe2+ has 6 negatron in its vitamin D orbitals while Fe3+ would hold 5 negatrons. The odd negatrons of the Fe ( III ) would hold a high spin and so act paramagnetically.
Fe2+ and Fe3+ negatrons can either administer themselves either in a low spin or a high spin agreement.
An illustration of the agreement which is more favoured harmonizing to Hund ‘s regulation
3d 4s 4p
3d 4s 4p
Iron can accept 6 braces of negatrons because the orbitals are hybridised in a manner to bring forth 6 orbitals of equal energy.
A redox titration is a type of reaction which is based on redox equations between the analyte and the titrant. Reduction-oxidation reactions are reactions where one of the constituent is being oxidized such as Fe ( II ) to press ( III ) therefore going more positively charged while the other is being reduced therefore it is deriving negatrons and will go less positive in its nature.
Potassium permanganate has the expression of MnO4- which can be reduced to Mn2+ in cut downing conditions. This is an oxidizing agent.
In this experiment the Fe ( II ) oxalate and K trioxalatoferrate ( III ) trihydrate were analysed. Then these two salts were analyzed for their Fe and oxalate content and besides the empirical expression of each salt was determined.
Apparatus: Pasteur pipette, weighing boat, spatula, ticker glass, mensurating cyclinder stirring rod, Buchner funnel, stopper, heating mantle, balance, beakers, thermometer, filter paper, ice-salt bath, flasks.
Method
Experiment A: Preparation of Iron ( II ) Oxalate
15g of ferric ammonium sulfate were dissolved in 50cm3 of warm H2O which has been acidified with 2M sulfuric acid ( 1cm3 ) .
75cm3 of 10 % oxalic acerb solution was added with rapid stirring. The mixture was heated gently to the boiling point and so the xanthous precipitate of ferric oxalate was allowed to settle.
The precipitate was removed by filtration on a Buchner funnel.
It was washed exhaustively with hot H2O and so with propanone.
The merchandise was allowed to dry on the funnel under suction and weighed.
The merchandise was used for the following subdivision.
Experiment B: Preparation of K trioxalatoferrate ( III ) Trihydrate
3.25g of ferric oxalate was suspended in a warm solution of K oxalate ( 5g in 15cm3 H2O.
15cm3 of 20vol H peroxide was added from a burette whilst the solution was stirred continuously and maintained at 40OC. The solution contained the precipitate of ferrous hydrated oxide.
This was removed by heating the solution to boiling.
10cm3 of 10 % oxalic acid and so a farther little sum of oxalic acid was added dropwise until the precipitate merely dissolved.
During the add-on of oxalic acid, the solution was maintained near the boiling point.
The hot solution was filtered.
15cm3 of ethyl alcohol was added to the filtrate, any crystals that were formed by soft warming were re-dissolved and put in a dark closet to clear.
The crystals were collected by filtration on a Buchner funnel.
These were washed with an equivolume mixture of ethyl alcohol and H2O and eventually with propanone.
This was dried, weighed and the merchandise kept in the dark.
Experiment C: The analysis of the merchandises for Fe and oxalate
Iron ( II ) oxalate
0.3g of oxalate was dissolved in 25cm3 of 2M sulfuric acid. The solution was heated to 60OC and titrated with 0.02M standard K permanganate solution until the first lasting tap coloring material was observed.
2g of Zn dust were added to the solution and boiled for 25 proceedingss.
It was filtered through the glass wall and the remainder was washed with 2M sulfuric acid.
The lavations were added to the filtrate and this was titrated with a solution of standard K permanganate
The per centums of Fe, oxalate, H2O of crystallization in the merchandise and the empirical expression were determined.
Potassium trioxalateoferrate ( III ) trihydrate
0.2g of the complex were dissolved in 25cm3 2M sulfuric acid. This was titrated with 0.02M standard K permanganate solution until the first lasting tap coloring material was observed.
2g of Zn dust were added to the solution and boiled for 25 proceedings.
This was filtered through a glass wool and the remainder was washed with 2M sulfuric acid.
The lavations were added to the filtrate and this was titrated with a solution of standard K permanganate.
The per centum of Fe and oxalate in the composite was determined.
These were compared to the theoretical values.
Precautions
The crystals were scraped from the filter paper which could take to inaccurate filtration.
The temperature of the solution was kept above 60oC during the titration of Fe oxalate against K permanaganate.
Titration setup was washed consequently ; Pipette and burette were washed foremost with H2O and so with the solution. Flasks were washed with H2O merely.
It was made certain that the burette was non leaky since it would impact the concluding consequence.
The merchandise of K trioxalatoferate ( III ) trihydrate was put in a dark closet since it is light-sensitive doing loss of merchandise.
A warming mantle was used alternatively of a Bunsen burner because ethyl alcohol is flammable.
When the ethyl alcohol was added to the filtrate in portion B the solution was left to chill down since if the ethyl alcohol was added to the hot filtrate the ethyl alcohol could hold evaporated.
Beginnings of mistake
- Glassware that was non calibrated decently could be a beginning of mistake
- The crystals were non dried wholly and so would take to higher weight.
- Loss of the merchandise due to reassigning from the balance to the flask, due to air currents and unsteady motions.
- The color of the terminal point could be misdirecting as different people have different sensitiveness to colors.
- Hydrogen peroxide could break up in light and so the oxidization of Fe ( II ) and Fe ( III ) would non be completed.
- Permanganate solution when allowed to stand in burette can undergo partial decomposition to MnO2.
- Difficult in seeing the measurings on the burette because of the dark violet produced by the permanganate solution
- Ferric ion is ruddy brown which could hold interfered with the observation of the swoon pink titration end point.
Discussion
Preparation of Fe ( II ) oxalate
When oxalic acid is added to the mixture of ferric ammonium sulfate in H2O and acidified with 2M of sulfuric acid, ions would organize in solution.
[ NH4 ] 2Fe [ SO4 ] 2.6H2O + H2O ® 2NH4+ + 2SO42- + Fe2+ 2
When adding oxalic acid to the solution oxalate ion signifiers which so reacts with the Fe ( II ) organizing the Fe ( II ) oxalic acid which is the merchandise. This is the xanthous precipitate which is removed by precipitation on a Buchner funnel. It is so washed with H2O and propanone to take drosss.
H2C2O4.2H2O + H2O ® 2H+ + [ C2O4 ] 2- 2
Fe2++ [ C2O4 ] 2- ® Fe [ C2O4 ] . 2H2O 2
Preparation of Potassium Trioxalatoferrate ( III ) Trihydrate
When K oxalate is added to the ferric oxalate an orange intermediate composite would be formed. During the readying of Potassium trioxalatoferrate ( III ) trihydrate the Fe ( II ) in the Fe ( II ) oxalate have to be oxidized to Iron ( III ) . This is done by an oxidizing agent which in this instance H peroxide is used. A brown precipitate of Iron ( III ) hydrated oxide would organize
2Fe2+ + H2O2 + 2H+ > 2Fe3+ + 2H2O 3
Fe3+ + 3OH- > Fe ( OH ) 3 3
This could be removed by extra warming. 10 % oxalic acid was added and so the oxalate ion could organize around the Fe ( III ) metal organizing a composite of Fe ( C2O4 ) . A green solution would organize in this phase. The undermentioned net equation would take topographic point change overing the Fe ( III ) oxalate to trioxalatoferrate ( III ) ion.
Fe2 ( C2O4 ) 3 + 3 H2C2O4 + 6 H2O > 2 [ Fe ( C2O4 ) 3 ] 3- + 6 H3O+ 3
The trioxalatoferrate ( III ) salt is soluble in H2O and would non precipitate out from an aqueous solution. Ethanol which is a less polar than H2O is added so that the salt would precipitate out since it is less soluble in ethyl alcohol. The precipitation is added by go forthing the mixture overnight so that the salt would precipitate. This is placed in the dark because visible radiation would cut down the Iron ( III ) to Iron ( II )
3 K+ + [ Fe ( C2O4 ) 3 ] 3- > K3 [ Fe ( C2O4 ) 3 ] 3
In the last portion of the experiment the per centum of Fe, oxalate and H2O of crystallization was found by titration of the Fe ( II ) oxalate with K permanganate which is the titrant. The volume of K permanganate needed to respond with the known volume of analyte was found. The titration was marked when a swoon tap coloring material appeared. This is the Mn2+ which serves as its ain index to demo when the titration is ready. In the first portion the oxalate and Fe ( II ) are both oxidized to Iron ( III ) and C dioxide. Zinc is added which acts as a reduction agent which reduces the Fe ( III ) back to Fe ( II ) .
When titrating the K permanganate with the K trioxalatoferrate ( III ) trihydrate salt, a swoon pink coloring material is observed when the stoichiometric point has been reached therefore titration would be completed. In the first portion the oxalate merely is oxidized to carbon dioxide since Fe ( III ) is already in its oxidised signifier. When Zn dust is added to the Iron ( III ) it is reduced to its reduced signifier Fe ( II ) .
The solution would stay colorless until all the oxalate salt is used. The solution is heated to 60OC since if the reaction takes topographic point at room temperature it would be excessively slow.
The oxidization of the oxalate anion which is an organic chelating agent, does non take topographic point really easy. In the presence of a metal ion, the rate of reaction additions since the oxidization would be kinetically more favorable when organizing an intermediate metal chelate. 4 In this experiment this type of intermediate had formed during the transition of the oxalate ion to carbon dioxide by the permanganate ion. 4 The permanganate ion is reduced to a lower oxidization province by taking an negatron from the oxalate and so the C C bond in the oxalate is broken organizing C dioxide.4
From the consequences one could detect that the per centums of Fe and oxalate in the theoretical output which are 31 % and 49 % severally are rather comparable to those per centums of the theoretical which are 31.89 % and 51.5 % . The theoretical per centum where brought by comparing the Fe and oxalate to the RMM of the Fe ( II ) oxalate. The theoretical % of H2O of crystallization in this compound is 20 % which resulted to be in close propinquity to the experimented value that of 16.6 % . When working the empirical expression of the oxalate Fe an estimate was taken and so it was non really accurate. The ratio of 1.02 was rounded to 1 and the ratio of 1.6 was rounded to 2 for the H2O of crystallization in the salt to ensue in the empirical expression of FeC2O4.2H2O
When working the per centums of Fe and oxalate in the K trioxalatoferrate ( III ) trihydrate the per centums were besides really near to the theoretical value since the % of Fe in the salt is 11.9 % when working the theoretical and the experimented values were worked to be 11.5 % . On the other manus, theoretically 56 % of the trioxalatoferrate ( III ) trihydrate is oxalate and 58 % oxalate in experimented value.
Decision
One can reason that the purposes were reached. The readying of these two compounds was done so that in the terminal the per centum of both Fe oxalate in the Fe ( II ) oxalate and the K trioxalatoferrate ( III ) trihydrate would be determined. The theoretical per centum of Fe and oxalate of the theoretical were about really near those that were determined by experimentation. The empirical expression of the Fe ( II ) oxalate was besides found to be FeC2O4.2H2O
