Basic Experiments

in Physical Chemistry

2022-1

Prof. : 한귀영 교수님

Student ID:
Name:
Assignment name: Lab #4 Result report
Date: 2022.03.22

Sungkyunkwan University
School of Chemical Engineering
 [Lab 4] Fractional Crystallization

1. Results

2.

alculation of the yield by calculating the theoretical value in the experiment and

comparing it with the obtained data

1) Calculation of the theoretically obtainable total potassium dichromate and sodium

chloride weights

Suppose that Na2Cr2O7·2H2O is a limiting reagent which reacts all with KCl, then we can

calculate the total mass of remained substances after the reaction like below.
Table 2. Representation of the reaction process and the number of moles and mass in

equilibrium using an ice table.

2) Calculate the yield of potassium dichromate (K2Cr2O7) and sodium chloride (NaCl)

and comparison with theoretical values

At the procedure 9, 1.1g of H2O was produced and (7+13) g of H2O already existed.

(∵7ml and 13ml of H2O were used and H2O density = 1.0 g/mL)

So the total mass of water is (7+13+1.1) g = 21.1 g.

Due to cooling in ice water, the solubility of K2Cr2O7 is 5 g per 100 g H2O at 0ºC and 1.06
g per 21.1 g H2O.

So, the actual theoretical mass of K2Cr2O7 is (8.83-1.06) g = 7.77 g.

In procedure 8, H2O evaporates and the total amount remaining is 1/4.

That is, the remaining H2O is (21.1/4)g = 5.28g.

As above, because of ice water cooling, the solubility of NaCl is 35.7 g per 100 g of H2O at
0ºC, and 1.885 g per 5.28 g of H2O.

So, the actual theoretical mass of NaCl is (3.506-1.885) g = 1.621 g.

Using the measured values in Table 1. and the calculated actual theoretical mass in Table 2.,

the yield of each material can be calculated.

As can be seen from Table 3 below, as a result of calculating the yields of potassium

dichromate (K2Cr2O7) and sodium chloride (NaCl), both were produced less than the

theoretical value.
3. Discussion about difference between original prediction and obtained data

1) Evaluation of Sodium Chloride Separation

When impurities are introduced into the reaction product, the yield may exceed 100%.

However, as a result of the experiment, the yield of NaCl was 82.85%, so it can be seen that

no impurities were added.

However, it cannot be said to be a complete success because there is a difference from the

yield of 100%.

2) Discussion of predictions and other acquired data

As mentioned above, a yield of 82.85% of NaCl and a yield of K2Cr2O7 (60.9%) were

calculated. In particular, it can be seen that the separation of K2Cr2O7 was not performed

well.

The errors mentioned below may have changed the mass and yield of the resulting product.

3) Possible errors

i) Assume that Na2Cr2O7·2H2O is the limiting reagent and all react with KCl

Contrary to the assumption, it is not known whether the limiting reagent has reacted 100% in
the experiment, so if the reaction is not completely terminated in the actual experiment, the

yield will be smaller.

ii) Assumption of solubility as a function of temperature

For yield calculations, it was assumed that K2Cr2O7 and NaCl dissolved in H2O at 0ºC

(cooled in ice water) and 100ºC (heated by heating plate), respectively. However, the

solubility depends on the temperature, and it was not considered whether the set temperature

was accurately maintained during the experiment.

iii) Consideration of the remaining amount in the experimental apparatus when

extracting the product

When transferring the solution to a flask, beaker, or Petri dish, a precipitate may remain in the

experimental apparatus in the previous order. This causes the yield to drop. Also, when the

solution is filtered with filter paper, some H2O may remain wet on the filter paper, affecting

the yield.

iv) Assumption of the amount of evaporated water

It was assumed that 3/4 of the total moisture content was evaporated during the course of the

experiment. However, it is not known exactly whether the amount of water remaining after

evaporation is 1/4. This will result in errors. If the amount of water remaining after

evaporation was less than the assumed value, the theoretical value would be larger than the

experimental value. If the amount of water remaining after evaporation was greater than the

assumed value, the experimental value would be larger than the theoretical value.

v) Consideration of the amount of water evaporated by heating during the

dissolution process
The solution is heated using a heating plate, which reduces the amount of water as it

evaporates. However, it is a cause of error because it is calculated that there is 13ml of

distilled water without considering this in the calculation

4) How to reduce errors

i) Rather than assuming that the limiting reagent reacts 100%, it is assumed that

more than 5% of the limiting agent remains in the actual experiment. Through

this, it is possible to correct the low calculated yield.

ii) When heating or cooling a solution, it measures the exact temperature at which

the temperature remains constant. The error can be reduced by measuring the

actual temperature and calculating the solubility.

iii) When transferring the solution to the flask-beaker-Petri dish, you can reduce the

error and increase the yield if you cleanly move the sediment remaining in each

experimental instrument or use more reagents.

iv) After filtration of the solution, the filter paper is dried to remove residual H2O.

5) K2Cr2O7 purification method including impurities

The K2Cr2O7 obtained after the experiment may also contain impurities. Contained

impurities can be purified through recrystallization, which uses the melting point difference.

The melting point of K2Cr2O7 is 398°C, and other impurities have higher melting points.

When the impure product dissolved in a selected solvent is boiled at the melting point of

K2Cr2O7 and cooled, only K2Cr2O7 can be crystallized. If this process is repeated, the

purity of the obtained material is increased, and K2Cr2O7 having almost no impurities can be

obtained.
4. Conclusion

1) The goal of the experiment

The goal of this experiment is to know the principle of separation of a solution mixed with

impurities using precipitation according to the difference in solubility between K2Cr2O7 and

NaCl, and to derive experimental values.

2) Analysis of experimental results

i) The measured values for the mass of K2Cr2O7 and NaCl can be obtained through

the experiment. The measured values for the mass of K2Cr2O7 and NaCl were

4.732 g and 1.343 g, respectively.

ii) Theoretical mass values of K2Cr2O7 and NaCl can be calculated using the

solubility value at a specific temperature, chemical reaction formula, and limiting

reagent information.

iii) The yield can be calculated by comparing the above-mentioned measured values

and theoretical values. The yields of K2Cr2O7 and NaCl were 60.90% and

80.85%, respectively.

Both materials yielded that were less than the theoretical values, but considering the factors

below, it will be possible to obtain a higher yield close to the theoretical value.

① In order to reduce the error, it is assumed that more than 5% of Na2Cr2O7 2H2O

remains in the actual experiment.

② During the cooling and heating process, while the temperature is kept constant,

the exact temperature of the solution is measured and calculated using the

solubility at that temperature.

 ③ When transferring from the laboratory equipment to another laboratory

equipment, avoid remaining sediment as much as possible, and use a larger

amount of reagents.

④ After filtering the solution, the filter paper is dried.

⑤ Consider the amount of water lost by evaporation during heating.

3) What we learned through this experiment

You can learn the factors that affect solubility and experiment with how to precipitate the

product from solution.

Using solubility, you can calculate the theoretical amount of the product and analyze the error

factors.

5. Answer for the result report

6. Reference

Sungkyunkwan University School of Chemical Engineering – (2020) Chemical Engineering

& Polymer Basic Experiments, p25-29

Physical Chemistry, p. Atkins, J de paula, 10th edition, p198-201

Libretexts

https://chem.libretexts.org/Bookshelves/
Physical_and_Theoretical_Chemistry_Textbook_Maps/

Supplemental_Modules_(Physical_and_Theoretical_Chemistry)/

Physical_Properties_of_Matter/Solutions_and_Mixtures/Case_Studies/

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