Experiment 5 EDTA Titration: Calcium in Calcium Supplements - CUHK [PDF]

EDTA Titration: Calcium in Calcium Supplements. Student Handout. Purpose. To determine the amount of calcium in a calciu

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Resource Book for Sixth-form Practical Chemistry

Experiment 5 EDTA Titration: Calcium in Calcium Supplements Student Handout

Purpose To determine the amount of calcium in a calcium supplement tablet by EDTA titration.

Background Calcium is an important element for our body. It is vital for the development of bones and teeth. More than 95% of calcium in our body can be found in bones and teeth. The long-term calcium deficiency leads to the decrease in bone density and strength. In fact, osteoporosis has affected many elderly people. To avoid this problem, calcium tablets may be taken to supplement the daily intake from diet. The calcium supplements consist mainly of calcium salts. Other ingredients are binders, colouring agents, flavouring agents, etc. In the present experiment, the amount of calcium in a supplement tablet will be determined by titration with a standard solution of ethylenediaminetetraacetic acid (H4EDTA). EDTA is commonly used as a chelating agent. It forms very strong 1:1 complex with most metal ions. The structure of H4EDTA is shown below. HOOCH 2C

H2 H2 C C N

N

HOOCH 2C

CH2COOH CH2COOH

As both the calcium ions and the calcium-EDTA complex are colourless, a suitable indicator that will change colour at the equivalence point has to be employed. Calmagite is used in the present experiment. It binds less strongly to the calcium ions than EDTA and exhibits different colours in free and bind forms at certain pH value. Ca2+(In)(aq) + EDTA4−(aq) (wine red)

Ca(EDTA)2−(aq) + In(aq) (blue)

where In stands for indicator.

29 Co-produced by The Chinese University of Hong Kong, Education and Manpower Bureau and Hong Kong Examinations and Assessment Authority

Experiment 5 EDTA titration: calcium in calcium supplements

Safety Handle all chemicals with great care. Avoid direct contact of chemicals with skin. Dispose of chemical waste, broken glassware and excess materials according to your teacher’s instruction. Safety information on the chemicals used in the investigation can be found in the Material Safety Data Sheet (MSDS). Consult your teacher for details.

EYE PROTECTION MUST BE WORN

Materials and Apparatus Available Calmagite indicator solution TOXIC

Standard 0.05 M EDTA solution HARMFUL/ IRRITANT

3 M HCl solution CORROSIVE

HARMFUL/ IRRITANT

CORROSIVE

HARMFUL/ IRRITANT

3 M NH3 solution

NH4Cl/NH3 buffer solution with Mg(EDTA)2− CORROSIVE

Burette Conical flasks Analytical balance Mortar and pestle

HARMFUL/ IRRITANT

Beakers Volumetric flasks Pipette Measuring cylinders

30 Co-produced by The Chinese University of Hong Kong, Education and Manpower Bureau and Hong Kong Examinations and Assessment Authority

Resource Book for Sixth-form Practical Chemistry

Experimental Procedure Photos of the experiment are available at http://www.chem.cuhk.edu.hk/ssc.htm. Make sure you have recorded all the observations and data. 1.

Preparation of sample solution Write down the information for the calcium supplement, especially the amount of calcium present in each tablet. Estimate the portion of tablet used for titration with ~25 cm3 of 0.05 M EDTA solution. Grind the tablet into powder. Weigh accurately the amount of powder needed and put it into a 250-cm3 conical flask. Add ~5 cm3 of 3 M HCl solution in small portions slowly to dissolve the powder.

2.

Titration with standard EDTA solution Add 50 cm3 of distilled water and 5 cm3 of 3 M aqueous NH3 solution to neutralise the final solution in Part (1). Add ~1 cm3 of buffer solution to obtain a pH value of ~10. Add a few drops of Calmagite indicator solution. The solution should be in wine red colour. Titrate with standard EDTA solution with continuous swirling until the wine red colour turns into blue. Repeat the titration twice.

Questions for Further Thought 1. 2. 3.

EDTA is not a primary standard. Suggest a method to standardise the EDTA solution. The present technique is employed to determine the hardness of water. Briefly describe what the hardness of water is and why we need to determine it. EDTA is used in chelation therapy. Describe briefly this treatment and the principle behind.

References 1.

2.

A. D. Eaton, L. S. Clesceri and A. E. Greenberg, Standard Methods for the Examination of Water and Wastewater, 19th Ed., American Public Health Association, Washington, 1995, pp. 2-35 - 2-38. http://web.centre.edu/che/che131_lab/calcium.html

31 Co-produced by The Chinese University of Hong Kong, Education and Manpower Bureau and Hong Kong Examinations and Assessment Authority

Experiment 5 EDTA titration: calcium in calcium supplements

Laboratory Report Form

Date: Title: Purpose:

Data and Calculation: Sample Information: Brand name: __________________ Amount of calcium per tablet (labeled): ___________ mg Weight of tablet: ___________ g Estimated weight of powder used: ____________ g Concentration of EDTA solution: ___________ M Trial 1

Trial 2

Trial 3

Weight of powder (g) Final reading of burette (cm3) Initial reading of burette (cm3) Volume of EDTA solution used (cm3) Calcium per gram of powder Average (g) % deviation

Amount of calcium per tablet: _____________ mg

32 Co-produced by The Chinese University of Hong Kong, Education and Manpower Bureau and Hong Kong Examinations and Assessment Authority

Resource Book for Sixth-form Practical Chemistry

Conclusions:

Questions for Further Thought 1.

EDTA is not a primary standard. Suggest a method to standardise the EDTA solution.

Answer:

2.

The present technique is employed to determine the hardness of water. Briefly describe what the hardness of water is and why we need to determine it.

Answer:

33 Co-produced by The Chinese University of Hong Kong, Education and Manpower Bureau and Hong Kong Examinations and Assessment Authority

Experiment 5 EDTA titration: calcium in calcium supplements

3.

EDTA is used in chelation therapy. Describe briefly this treatment and the principle behind.

Answer:

34 Co-produced by The Chinese University of Hong Kong, Education and Manpower Bureau and Hong Kong Examinations and Assessment Authority

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