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Chemistry 101 PRAC A The fertiliser sample was diluted with de-ionised water to dissolve as much of the sample

as possible. 3mL of 2M HCl was mixed with the solution, which served to break apart the bonds connecting the sulphate ions in the fertiliser. The reaction was probably represented like so: ?SO42-(aq) + HCl H? + Cl? + SO42-(aq) The solution of HCl and fertiliser is boiled to catalyse the speed of the reaction. Drop by drop, a process which ensured a precipitate, 15mL of 0.5M BaCl2 was added with a burette in excess. A white precipitate was formed. The reaction of the precipitate forming was: Ba2+ (aq) + SO42- (aq) BaSO4(s) This solution was boiled in order to catalyse any reactions. To make sure that there was no further SO42- in the solution, an additional 3mL of 0.5M BaCl2 was added. The solution was left overnight for the BaSO4 to form and cool down slowly. In order to separate the precipitate (BaSO4) from the solution, the solution was vacuum pumped, gently, through filter paper. The process was repeated until the was a satisfactory level of BaSO4 not present in the remaining solution. The precipitate was weighed and found to be 1.2g. This process is known as gravimetric analysis. In order to find the mass of the sulphate ions present in the precipitate. 1 2 3 But when determining the percentage of mass of the sulphate in the fertiliser. 1 2 3 Also when determining the percentage by mass of sulphur (as sulphate) in the fertiliser. 1 2 3 Possible sources of error that are present in the equation could be. 1. Loose hair or cotton from the performers of the experiment, this could add excess weight to the solution, precipitate and/or powder and effect the overall result. 2. When the precipitate is collected in the filter paper, the paper is not fine enough to catch it all. This could effect the end result be lowering the amount of precipitate weighed. The commercial percentage is different because large companies will perform the experiment multiple times to ensure a generalised, universal result. Also, the fertiliser which was used was old, meaning that it is possible some of the nutrients may have compacted down to the bottom of the bag, leaving less on the top.

PRAC B NH4+ is not a very strong acid, so it doesnt give a sharp end point, or colour change, when titrating. Therefore, several samples of fertiliser solution were diluted with de-ionized water to dissolve the fertiliser. The container with the solution was swirled to thoroughly mix the two compounds. 20mL of the solution was added to three volumetric flasks. 20mL of 0.09897M NaOH was added, via pipette, in order to separate some of the bonds between the fertiliser and its NH4 molecules. This process however is not accurate given the nature of filling and emptying the pipette. The equation of this process is shown as: NH4+ (aq) + OH-(aq) NH3 (g) + H2O (l) When boiled, the NH4+ in the solution evapourated. To show all the NH4+ in the solution evapourated, red litmus paper held into the steam, which came out of the conical flask, stayed red, not turned blue as an acid would show. Once this was completed, the remaining solution was titrated with enough 0.10256M HCl to warrant a change of colour. The equation to represent this process was: NaOH (aq) + HCl (aq) NaCl (aq) + H2O (l) The results were as follows: Titration Initial Burette Reading 1 0.00mL 2 9.2mL 3 18.2mL Final Burette Reading 9.2mL 18.2mL 27.2mL Titre (mL) 9.2 9.0 9.0

The excess NaOH in the solution is calculated compared to the amount of HCl added. From there the amount of NH4 is calculated from the NaOH. This process is known as Back Titration. To find the amount of NaOH, in mol, in each sample: 1 2 The average titre of HCl would be: 1 2 The amount of HCl used in the titration is shown as: 1 2 The amount of NaOH that did not react with the fertiliser in each solution would be: 1 2

PRAC B The amount of NaOH that reacted with the fertiliser: 1 2 The amount of NH4 in each sample mixed that mixed with the NaOH: 1 2 The original amount of NH4 present in the 250mL flask: 1 2 The mass of N in the fertiliser: 1 2 3 The percentage by mass of nitrogen in the sample: 1 2 The result of the experiment showed that there was a higher concentration of Nitrogen in experiment then in the commercial results. This could be to inaccurate amounts of NaOH or HCl being added to their respective solutions, which would affect the results marginally. Also, when the HCl was added to the solution of NaOH and NH4 deprived fertiliser, there may have been more than just NaOH reacting with the HCl which would have caused results to be higher.

PRAC C Iron, being a transition metal, can have different states of oxidation. Given this attribute, a titration against KMnO4 can reveal how much Iron, Fe, is in a solution. In a titration between these two compounds, involving oxidation and reduction, the appropriate equations of oxidation and reduction were: Oxidation: Fe2+ Fe3+ + eReduction: MnO4 +8H =5e- Mn2+ + 4H2O Combining to equal: 5Fe2+ (aq) + MnO4 (aq) + 5e- Mn2+ (aq) + 5Fe2+ (aq) +4H2O (l) Though in order to get the H ions into the solution, 20mL of 1M H2SO4 had to added. Additionally, no indicator needed to be added to the KMnO4 as it is a deep purple colour, which turned colourless as the 1.0M HCl was added; furthermore, when the KMnO4 was measured, it was to be measure above the meniscus, a change from the usual method of measuring to below, as it was too dark to clearly see the line. 10g of fertiliser was mixed with 100mL of de-ionized water to dissolve the fertiliser into a solution. The solution was swirled/inverted until there was a satisfactory amount of dilution; then filtered through grade 4 filter paper, which would remove any insoluble compounds in the solution. 20mL of 1.0M H2SO4 was added to the solution to assist in adding Hydronium atoms, a necessary element in the redox titration which occurred. 20mL of 0.01M KMnO4 was added to a conical flask as a standard solution. 200mL of de-ionized water was added to the fertiliser solution. Drop by drop, helpful for calculating exact colour change, the fertiliser solution was added to the KMnO4 until a colour change was observed. This was repeated 3 times for concordant results. The results of the titration were as follows: Titration Initial Burette Reading 1 5 2 9 3 12.5 4 16 Final Burette Reading 8.9 12.5 16 19.6 Titre (mL) 3.9 3.5 3.5 3.6

PRAC C The iron content in the fertiliser as percentage by mass was: 1 2 3 4 5 6 Possible sources of error which could have occurred during the experiment could be: 1. If there were other compounds in the fertiliser which could be oxidised by the permanganate ions, the result would be adversely affected as the percentage of Fe in the solution would appear higher. 2. Incorrect labelling in the concentration of the chemicals may have led to a miscalculation when the percentage was being counted up. The manufacturers specifications stated that there was 1.1% iron in their product, though the experiment and calculation claimed there was 4.1%. This could be due to other compounds which were not filtered properly oxidising with the permanganate ions or labelling errors on the bottles, not giving the correct concentration.

PRAC D

In order to find the concentration of PO43- ions in the fertiliser sample, the following equation must be used to find the amount of sample needed for a 250mL solution: 1 2 3 20mL of hot, de-ionized water was added to the 1g sample of fertiliser in order to break down the samples PO43- bonds. The solution was then increased to 250ml by adding deionized water. Furthermore, the solution was diluted by a factor of 10 by taking 25mL of the solution and increasing it to 250mL. 20mL of the solution was added to a test-tube labelled unknown. Additionally a respective amount of solution and de-ionized water was added to test-tubes named in the following graph: Test-tube label (mg.L1) Volume of phosphate solution (mL) Volume of water (mL) 10.0 20 0 7.5 15 5 5.0 10 10 2.5 5 15 0.0 0 20 To show indicate when a change occurred in the experiment, 2mL of ammonium molybdite reagent was added; as was a few crystals of ascorbic acid. The ammonium molybdite reagent caused the phosphates to be converted to phosphomolybdate. The reaction was similar to this: (NH4)3PO4 (aq) + 12(NH4)2MoO4 (aq) + 24HNO3 (aq) (NH4)3PO4.12MoO3 (aq) + 24NH4NO3 (aq) + 12H2O (l) The resulting (NH4)3PO4.12MoO3, phosphomolybdate, was then reduced to phosphate by then ascorbic acid. The six test-tubes were added to 200mL of boiling water at exactly the same time, being added at exactly the same time was necessary as it allowed universal time to catalyse the reaction. The solutions would turn blue, as the ascorbic acid reduced the phosphomolybdate into molybdite blue and phosphate. After ten minutes, the test-tubes were removed, at the same time, and placed one by one into a colorimeter. The colorimeter measured the absorbance of light in the phosphate and produced the results as follows: Standard (mg.L-1) 10.0 7.5 5.0 2.5 0.0 Unknown PRAC D Absorbance 3.11 2.59 2.51 1.66 1.06 2.49