Stage 2 Chemistry Volumetric Analysis Practical

Assessment Exemplar Assessment Component 3: Practical Work

Background: Iron(II) ammonium sulfate is also known as Mohrs salt. Mohr was a German chemist who specialised in volumetric analysis. Many iron(II) compounds oxidise on exposure to air making them difficult to use in volumetric analysis. It was found that the iron(II) ion in iron(II) ammonium sulfate was more resistant to oxidation than other iron(II) compounds. The formula of Mohrs salt is Fe(NH4) 2(SO4) 2.6H2O and its molar mass is 392.16g mol-1. The equation for the titration in the following practical is:
-

5 Fe 2+ + MnO4

+ 8 H+

5 Fe 3+ + Mn 2+ + 4 H2O

Aim: You will be provided with a pre-weighed sample of Mohrs salt. The sample will have a mass between 7.700g and 8.100g. You are to determine this mass by using the titration procedure outlined. (Weighing is not allowed!) Different sample numbers have different masses of Mohrs salt. Materials: Labelled sample of Mohrs salt Procedure: Part A: Preparing a solution of your Mohrs salt sample using a volumetric flask. Note: The mass of your sample has been carefully pre-weighed to the third decimal place. You wont know the concentration of your solution until the final calculation, but its correct mass and the expected titre values are known by your teacher. It is critical that all of the Mohrs salt is transferred then dissolved. Concentrated sulfuric acid 2.00 mol L-1 sulfuric acid solution 150 mL standardised 0.0200 mol L-1 potassium permanganate solution a range of volumetric flasks 100 mLbeaker 20.0mL pipette and pipette filler burette 250 mL conical flasks burette funnel white tile retort stand and clamp

The sample contains approximately 8 g of salt and the solution you make will need to have a concentration of approximately 0.1 mol L-1. Find by calculation the best size volumetric flask to use. Transfer your sample into a clean rinsed 100mL beaker. Use distilled water to rinse out any remaining solid from the container into the beaker. Completely dissolve all of the salt in an appropriate volume of distilled water. Carefully transfer the solution to your chosen volumetric flask. Ensure that all the salt is transferred to the flask by rinsing the beaker several times, and adding the rinsings to the volumetric flask. Add 5 drops of concentrated sulfuric acid to the solution. Add distilled water to the calibration mark.
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Stopper and mix the solution thoroughly

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Part B: Titration using a potassium permanganate solution of known concentration, to determine the concentration of your standard Mohrs salt solution. Rinse the burette appropriately and then fill it with the 0.0200 mol L -1 potassium permanganate solution. Use a rinsed pipette to transfer 20.00mL aliquots of your standard Mohrs salt solution to a 250.0mL conical flask. Use a measuring cylinder to add approximately 20mL of dilute (2.0 molL -1) sulfuric acid. Add potassium permanganate solution from the burette until the titration end point is reached. Carry out a rough titration first, then accurate titrations until concordant titres are obtained. Enter all results on the table provided: Hand in your record sheet to your teacher to have it signed

Calculations and report: Use the results from your titration to calculate the concentration of your Mohrs salt solution. Find the mass of Mohrs salt used in your solution, using the concentration calculated and the molar mass of Mohrs salt, See your teacher to obtain the pre-weighed mass for your sample. Record this on your results sheet. Write a report showing your calculations and addressing the criteria outlined on the mark scheme under interpretation and evaluation SAFETY FIRST

Safety glasses and

aprons must be worn.

Wash your hands after completing the practical.

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STAGE 2 CHEMISTRY STUDENT _________________________ RECORD SHEET

VOLUMETRIC ANALYSIS PRACTICAL

Part A: Preparing a solution of your Mohrs salt sample using a volumetric flask.
Sample No:___________________ Volumetric flask size:__________________

Part B: Titration
Concentration of potassium permanganate solution:___________________ Volume of pipette used:________________ Volume of sulfuric acid used:__________________

Titration Number final volume (mL) initial volume (mL) Titre (mL)

Average titre:

Teachers Signature:_______________________________ Date:_________________________

Pre-Weighed mass:__________________________

SSABSA Support Materials: 184306240.doc, last updated 16 April 2008

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STAGE 2 CHEMISTRY STUDENT _________________________

VOLUMETRIC ANALYSIS PRACTICAL

MARKS SCHEME (To be submitted with the signed record sheet and the practical report)
Maximum Mark

Mark

Teachers Comment

practical skills
Select and use glassware of appropriate resolution for making solution Select and correctly use apparatus: 1. volumetric flask 2. volumetric pipette 3. burette. Concordance of titres: within 0.1(within 0.2) 2

1 1 1 2 (1) 2

presentation
Record and use measurements to an appropriate number of significant figures.

interpretation and evaluation

Use data to perform calculations for: Concentration of Mohrs salt solution Mass of Mohrs salt Identify sources of and distinguish between random and systematic errors Identify random error source and explain how to minimise. Identify possible systematic error source and explain how to detect. Critically analyse and evaluate experiment and suggest improvements. Explain why an approximate volume of sulfuric acid is acceptable. Describe and explain rinsing procedures for pipette and burette. Suggest two improvements Discuss the precision and accuracy of the result Draw a valid conclusion 1 2 2 2 1 1+2 1+2 4 3

communication Present information logically TOTAL: 2 32

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SSABSA Support Materials: 184306240.doc, last updated 16 April 2008