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Risk Assessment

0.05 M EDTA , 3M HCl, 3M NH3, buffer solutions are harmful, so we must


handle them with great care. Three chemicals used: 3M HCl, 3M NH3, and
NH4Cl/NH3 buffer solutions are corrosive. We must avoid direct contact of
chemicals with skin ;otherwise, we may get skin burn and feel sting.
Furthermore, we need to wear safety glasses to protect our eyes and wear
protective gloves to protect our hands.

The buffer solution has a very strong smell of ammonia, so keep the buffer
solution bottle closed to avoid inhale to much of the ammonia smell.
If any chemicals are splashed onto our skin or clothing, we should wash the
affected area immediately with slow running water.
As the chemicals are corrosive, we should dispose of chemical waste with our
teacher’s instruction.

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Procedure
1. Set-up
I. Take out a stand and clamp.
II. Clamp the burette
III. Add 50cm3 of the EDTA solution by using a filter funnel.

2. Preparation of sample solution


I. Grind the tablet into powder with mortar and pestle.

II. Weigh 0.01g of the powder on the analytical balance. Pour it into a
conical flask
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III. Measure 5cm3 of 3M HCl solutions with measuring cylinder. Take
the reading at eye level.

IV. Add the 3M HCl solutions slowly to


dissolve the powder.

3. Titration with EDTA solution


I. Use a pipette to hold 50cm3 of distilled water. Measure 5cm3 of 3M
NH3 solutions with measuring cylinder.
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II. Add the distilled water and the NH3 solution to neutralize the final
sample solution.

III. Pour a certain amount of buffer solution into a beaker.

IV. Measure 1cm3 of buffer solution with measuring cylinder.

V. Add this to obtain a pH value of about10


VI. Add 3 drops of Calmagite indicator
solution. The solution should be wine
red.
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VII. Titrate with standard EDTA solution with swirling till the solution colour
changes to blue.
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Results and calculations


Sample information:
Amount of calcium per tablet (labeled): 200 mg (0.2g)
Weight of tablet: 0.97g
Weight of powder used: 0.01g
Concentration of EDTA solution: 0.05M
Trial 1 Trial 2 Trail 3 Trial 4

Initial reading 0.00 0.00 0.00 0.00


of burette
(cm3)
Final reading 5.10 4.00 3.70 3.50
of burette
(cm3)
Volume of 5.10/1000= 4.00/1000= 3.70/1000= 3.50/1000=
EDTA solution
0.0051 0.0040 0.0037 0.0035
used (dm3)

Average(dm3) 0.0051+0.0040+0.0037+0.0035)/4

= 0.004075

Molarity of EDTA solution = No. of moles of EDTA / volume of solution


0.05 = No. of moles of EDTA/0.004075
No. of moles of EDTA =2.0375 x 10 -4mol
Mass of calcium in 0.01g of powder = 0.00020375 x 40.1
= 8.170375 x 10 –3 g
Mass of calcium per tablet = [8.170375 x 10 –3 (0.97/0.01)]g
= 0.7925
=0.793g (cor. to 3 sig. fig)
Percentage by mass of calcium per tablet:
(0.7925g/ 0.970g) x 100%
= 81.7%

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Discussion
After the experiment, we have noticed that the mass of calcium per tablet
was much bigger than the labeled (0.2g).

We have founded several sources of errors. First, the calcium tablet


contains calcium carbonate but also magnesium oxide. The Ca2+ will
combine with EDTA 4- at a pH of about 10 and Mg 2+ will do this at a pH
greater than 12. When we had measured the hydrochloric acid in a
measuring cylinder, we had left it exposed to air for a few minutes. As
concentrated hydrochloric acid gives acid mist, loss in mass might be
resulted .So, the pH value of the sample solution might be greater than 12,
as a result, the amount of calcium calculated might have included that of
magnesium. We should control the pH value of the sample solution strictly
by using the pH meter to measure and we should add the hydrochloric acid
to the solution just after measuring.
Furthermore, we probably had added excess EDTA solution, which
means we couldn’t stop titration immediately when the end-point of the
titration had reached. The volume of EDTA solution used might be greater
than expected amount. Next, we hadn’t cleaned the measuring cylinder and
dropper completely before next measurement. The solution might be
contaminated with the last chemical used. Therefore, we should clean the
measuring cylinder and dropper through before each measurement. The
contamination of the solutions can be reduced.
Conclusion
After calculation, 0.793 g of calcium can be founded in per tablet. The
percentage by mass of calcium per tablet is 81.7%. Thus, this calcium tablet
can really supplement the dietary intake.

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References
CHEMISTRY 221 LABORATORY—QUANTITATIVE ANALYSIS
http://www.cofc.edu/~kinard/221LCHEM/CHEM221L%20Calcium%20Determi
nation%20by%20EDTA%20Titration.htm

Calcium Determination Using EDTA


http://home.snu.edu/dept/chemistry/syllabi/ARCHIVES/CHEM3024/Labs/LAB
4%20-%20Ca_edta.htm

Testing Calcium Carbonate


http://www.wcaslab.com/tech/Calcium_Carbonate.htm
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