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Lesson 2 Solid Purification

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6 views

Lesson 2 Solid Purification

hay

Uploaded by

Huy Nguyễn
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Lesson 1

SOLID PURIFICATION: BENZOIC ACID PURIFICATION BY


RECRYSTALLIZATION

Chemical
Crude benzoic acid : 5 grams
Distilled water : 210 ml
Activated carbon : 0.1 grams

Tool and apparatus


Electric stove : 1 pc
250 ml single-neck round bottom flask (joint 29/32) : 1 pc
Bulb condenser (joint 24/29) : 1 pc
100 ml Glass beaker : 1 pc
50 ml Glass beaker : 1 pc
Glass drying dish : 1 pc
Stir rod : 1 pc
Melting point apparatus : 1 set
Vacuum filtration apparatus : 1 set
- Clamp, balance, chemical measuring cylinder, capillary tube, vacuum grease.
Procedure
1. The equipment is installed as shown in Figure 1:

Figure 1: Diagram of making a saturated benzoic acid solution


- The bulb condenser in the flask in the straight position standing,
- The bottom of the flask is about 2-3cm from the electric stove.
- Let the water flow through the bulb condenser
2. Making a saturated solution of benzoic acid

- Add 5 grams of benzoic acid and 210 ml of water


- Store in a 250 ml single-neck round bottom flask (29/32)
- Plug in the power and proceed to create a solution saturated benzoic acid.

During the refluxing process, observe the dissolution of benzoic acid:

- When the solution in the flask boils for about 5 minutes, If there is a lot of solids,
add a little more drop of water through condenser (note: turn off the electric stove
before adding water).
- Then, let the boiling process continue until the solid dissolves completely. The
solution is saturated in the flask at boiling point of water.

If there is color, it must be removed. How to remove the color:

- Turn off the electric stove,


- Let the flask cool down for a while,
- Then remove the bulb condenser and add in the flask about 0.1g of activated
carbon finely grounded.
- Then fit the bulb condenser and reflux again the mixture.
3. Filter and dry
- The hot solution after bleaching color is filtered to remove insoluble impurities by
a vacuum filtration apparatus (Figure 2)

Figure 2: Vacuum filtration apparatus


A hot, transparent and colorless solution is obtained. (note: this step needs to be
carried quickly to avoid recrystallization in the flask).
- The resulting solution is divided into 2 beakers: One beaker is capped, let stand at
room temperature. One beaker is quickly cool by ice outside while stirring by stir
rod at the same time.
- Trace crystals appear in both beakers, please compare two observed crystals in
different recrystallization methods and write conclusions.
- Then, combine the crystals in both beakers and cool with ice outside, then filter
out the crystals by vacuum filtration apparatus. Wash the crystals immediately on
the Buchner funnel with a small amount of cold water.
- Obtained product was dried at 80oC until dry. When the product is completely
dry, determine the melting point (Figures below). Weigh the dry product obtained
and calculate the yield.
- Pure benzoic acid is a colorless crystalline solid with a melting point of 122.4oC.
The process of melting point measurement as follow:

1. Seal the cappillar tube

2. Stuff benzoic acid into capillary tube


3. Melting-point measurement of benzoic acid using melting point apparatus
EXPERIMENT REPORT
LESSON 1: SOLID PURIFICATION: BENZOIC ACID PURIFICATION BY
RECRYSTALLIZATION

Student's full name: …………………………………… ……………………………


Student code: ……….. …Group:
Instructors: ………………………………………………………………………
Experiment date………………………………………………………………………..
Evaluation of instructors

1. Physical, chemical and application properties of benzoic acid:

2. Principle of recrystallization method:

3. Chemicals used:
4. Draw the implementation diagram (figure) and explain:

5. Purpose and method of bleaching:


5.1 Purpose:

5.2 Method:

6. Compare the benzoic acid crystals formed under 2 conditions (standed at room
temperature and stir, cooled by ice outside). Explain?

7. Describe filtering methods:


7.1 Filter the solution:
7.2 Filter for crystals:

8. Why are crystals of benzoic acid dry at 80oC?


when do you stop drying benzoic acid?

9. Compare the actual melting point of benzoic acid with your practical melting
point measurement by apparatus. Explain?

10. Experimental results:


Mass of acid used: m1=…………. (g); Mass of acid obtained: m2=………… (g)
Melting temperature: t1 =……………………. (oC) ; t2 = ………………… (oC).
Purification efficiency: …………………… (%).

Instructor Laboratory technician Student


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