Limiting reagent synthesis of CaCO3

Introduction and Goals

Experiment 3: Limiting reagent synthesis.

Date: 20 September 2023

Name: Albane Fery

Lab Partner: Joe Robinson

Introduction

 The aim of this experiment is to predict the limiting reagent and resulting theoretical yield for the formation
of CaCO3.
 Following the isolation of the final product, we will then be able to calculate the actual yield and
percentage yield.

Lab safety

 Na2CO3 and CaCl2 pose minimal hazards – wear goggles to prevent solutions from getting into eyes, as well
as gloves and a lab coat.
 Glassware used is fragile – if glassware breaks, broken pieces can be hazardous.

Materials

 Na2CO3 and CaCl2 solids

 Volumetric flasks
 Burettes
 Distilled water
 Waste beaker
 Reaction beakers
 Filtration flask
 Buchner funnel
 Filter paper
 Weighing boats
 Stir plate & stir bars.
 Laptop with Excel software to record data.

Methods
Complete lab protocol: https://wakeforest.instructure.com/courses/56305/files/3707658?module_item_id=1204135

1. Preparation of reagents
a. Weigh out the calculated masses of Na2CO3 and CaCl2 solids needed to create 0.2M solutions.
b. Put each solid into a separate volumetric flask and fill these up to the 100 mL marker with distilled
water, making sure both solids are dissolved – make sure to measure the 100 mL marker from the
bottom of the meniscus.
c. Rinse a burette (labelled CaCl2) with water and then the calcium chloride solution – fill the burette
above 0 mL with the solution and purge any air bubbles in the tip by draining a small amount of
the solution into the waste beaker.
d. Rinse a second burette (labelled Na2CO3) with water and then with the sodium carbonate solution
– as before, fill the burette to above 0 mL with the solution, and drain to purge any air bubbles.

Reaction Volume of CaCl2 (mL) Volume of Na2CO3 (mL)

1 12.00 18.00

2 13.00 10.00

3 10.50 10.20

Fig. 1. Table showing the reaction volumes for each solution in each individual reaction.

2. Synthesis
a. Fill the burettes with enough solution for each reaction.
b. Using the reaction volumes in Figure 1 above, fill each reaction beaker with the planned volume
of solution.
c. Once the solutions are added, stir each reaction mixture on a stir plate for 2 minutes.
3. Isolation of product
a. Determine and record the mass of the piece of filter paper (for each reaction mixture).
b. Using a filtration flask, Buchner funnel and the weighed filter paper, filter the contents of each
reaction beaker – use distilled water to quantitively transfer as much of the solid as possible into
the funnel.
c. Rinse any product left on the stir bar into the Buchner funnel using distilled water
d. Weigh and label 3 weighing boats (one for each reaction mixture) and transfer the filter papers
with the product on them into each boat.
e. Leave the products to dry in the lab for the next 7 days.
4. Determining mass of final product
a. When the contents have dried, determine, and record the mass of the product by subtracting the
mass of the weigh boat and filter paper from the final mass.
Observations

Fig. 2. Images showing the solutions before and during mixing.

As soon as the Na2CO3 and CaCl2 solutions came into contact with each other, the solution became cloudy and
white, and a precipitate formed. All three solutions had a similar color, with the cloudiness appearing only once the
solutions came into contact with each other.

Data

Preparing stock solutions:

Molecular weight of CaCl2 – 110.98 g/mol

Molecular weight of Na2CO3 – 105.99 g/mol

CaCl2 Na2CO3

Moles needed for 0.200 M (mol) 0.2 x 0.1 = 0.0200 0.2 x 0.1 = 0.0200

Mass needed for 0.200 M (g) 0.0200 x 110.98 = 2.2196 0.0200 x 105.99 = 2.1198

Actual Mass Used (g) 2.2206 2.1138

Actual Moles (mol) 2.2206 / 110.98 = 0.0200 2.1138 / 105.99 = 0.0199

Actual Molarity (M, mol/L) 0.0200 / 0.1 = 0.2001 0.0199 / 0.1 = 0.1994

Fig. 3. Calculations involved in preparing stock solutions.

Reactions:

Reaction 1 Reaction 2 Reaction 3

 Volume of CaCl2 added 12.0 13.0 10.5
(mL)

Moles of CaCl2 added 0.2 x (12.0 / 1000) = 0.2 x (13.0 / 1000) = 0.2 x (10.5 / 1000) =
(mol) 0.0024 0.0026 0.0021

Volume of Na2CO3 18.0 10.0 10.2

added (mL)

Moles of Na2CO3 added 0.2 x (18.0 / 1000) = 0.2 x (10.0 / 1000) = 0.2 x (10.2 / 1000) =
(mol) 0.0036 0.0020 0.0020

Fig. 4. Calculations involved in determining the contents of the reaction mixtures.

Reaction 1 Reaction 2 Reaction 3

Moles of limiting 0.0024 0.0020 0.0020

reagent (mol)
(CaCl2 limiting) (Na2CO3 limiting) (Na2CO3 limiting)

Moles of Ca2+ in excess 0 0.0006 0.0001

(mol)

Moles of CO32- in excess 0.0012 0 0

(mol)

Theoretical yield (mol) 0.0024 0.0020 0.0020

Theoretical yield (g) 0.0024 x 110.98 = 0.2664 0.0020 x 105.99 = 0.2120 0.0020 x 105.99 = 0.2162

Fig. 5. Calculations involved in determining the theoretical yield from the three reaction mixtures.

Reaction 1 Reaction 2 Reaction 3

Isolated mass of product 2.7804 – 2.5361 – 0.1764 2.9355 – 2.5959 – 0.1716 2.8567 – 2.4989 – 0.1777
(g) = 0.0679 = 0.1680 = 0.1801

% yield (%) (0.0679/ 0.2664) x 100 = (0.1680/ 0.2120) x 100 = (0.1801 / 0.2162) x 100 =
 25.5 79.3 83.3

Fig. 6. Calculations involved in finding the percentage yield of the reaction.

Results

Reaction 1 Reaction 2 Reaction 3

Theoretical yield (g) 0.2664 0.2120 0.2162

Isolated mass of product 0.0679 0.1680 0.1801

(g)

% yield (%) 25.5 79.3 83.3

Fig. 7. Table showing the final, key results of the experiment.

Fig. 8. Images showing the white

precipitates formed in each reaction.

Discussion

The results shows that the highest percentage yield occurred from reaction 3, with 83.3% of the theoretical yield of
product being formed. Reaction 1 produced the smallest percentage yield, with only 25.5% of the theoretical yield of
product being formed.

There are many reasons for why a reaction may generate a low percentage yield. An obvious one as we were
conducting the experiment was loss of product. When pouring the solution onto the filter paper, we could see rings
of white product left on the beaker even once we had poured all the solution out and rinsed the beaker. This suggests
that product was left in the beaker and not transferred onto the filter paper, reducing the final isolated mass of
product and therefore the percentage yield.
Fig. 9. Image showing the white rings of product left in the beaker even after rinsing, suggesting loss of product.

Another reason for our low percentage yield could also have been uncertainty in our measurements. When recording
volumes from our burettes, the digit estimates between the smallest graduations were only to 2 decimal places, with
the value being to the nearest 0.05, and this was measured qualitatively using eyesight, so there was a margin for
error. This could have meant that our volume measurements were slightly skewed, affecting the reaction and
limiting reagent, and therefore the reaction yield.