University Of Central Lancashire Department of Forensic and Investigative Science FZ1025 Experimental Techniques in Chemistry

8. Determining the hardness of water via EDTA-titration

INTRODUCTION The hardness of water is conventionally expressed in three parts: 1. Total hardness, which is determined by the total amount of magnesium and calcium containing compounds present in water. 2. Permanent hardness, which is determined by the amount of magnesium and calcium containing compounds present in water after boiling the water. Boiling the water may cause the formation of solid calcium carbonate, which may be removed by filtration. 3. Temporary hardness, which is calculated by subtracting the value of permanent hardness from the total hardness. The hardness of water is expressed in mg CaCO3 per litre of water. PRE-LAB QUESTIONS 1) Draw the structure of EDTA 2) How does EDTA bind with metal ions like calcium or zinc? 3) Discuss some of the current methodologies for softening water. (2 marks) (3 marks) (5 marks)

HEALTH & SAFETY Chemical / Process Hazard Severity Grade 1-4 A

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Likelihood of occurrence Grade 1-4 B

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Risk (A x B) (Likelihood x hazard)

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Safety

Zinc acetate dihydrate

EDTA dilute solution, -1 0.01 mol l Ammonia buffer Eriochrome black T solution (dilute)

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Harmful by ingestion/inhalation. Wash with copious amounts of water for at least 15 minutes and consult a physician. Irritating, wash with copious amounts of water. Irritating, wash with copious amounts of water. Harmful, wash with copious amounts of water.

EXPERIMENTAL Standardisation of 0.01 M EDTA against zinc acetate dihydrate. 1. Perform the standardisation of the 0.01 M EDTA-solution with zinc acetate dihydrate. Calculate the mass of zinc acetate dihydrate (M=219.51 g.mol-1) required in order to use approximately 25 ml of EDTA-solution. 2. Dissolve the zinc acetate in 100 ml E-pure water, transfer to a conical flask quantitatively, add 2 ml ammonia buffer pH=10, 5 drops of ERIO-T indicator and titrate whilst stirring until colour change from wine red to blue occurs. 3. Repeat twice and calculate the average concentration and standard deviation. Determine the hardness of all water samples in duplicate, according to the following procedure: The permanent hardness of water 1. Transfer 100.00 ml sample to a 500 ml beaker and bring to a boil for 10 minutes, place a watch glass on top of the beaker to prevent evaporation of water. 2. Allow to cool to room temperature (continue with the determination of the total hardness of water). 3. Filter the water into a 250 ml conical flask, add 2 ml buffer solution and 5 drops of ERIO-T indicator. 4. Add a magnetic stirrer and heat the solution to 70C (make sure the temperature is stable) and titrate with 0.01 M EDTA. Titrate slowly when you see the colour of the solution starting to change. When the colour is stable (clear blue) for 20 seconds, you have reached the end-point. The total hardness of water 1. 50.00 ml sample in 250 ml conical flask 2. Add 2 ml buffer solution (ammonia pH=10) and 5 drops of ERIO-T indicator. 3. Add a magnetic stirrer and heat the solution to 70C (make sure the temperature is stable) and titrate with 0.01 M EDTA. Titrate slowly when you see the colour of the solution is starting to change. When the colour is stable for 20 seconds, you have reached the end-point.

POST-LAB QUESTIONS 1. Report the average concentration for the EDTA-solution and show your workings in one example 2. Report the calcium concentration in all water samples (show your workings in one example) and discuss any differences. 3. Calculate the total, permanent and temporary hardness of water in mg CaCO 3 per litre and show your workings