Extraction (Part 2) Experiment: Separation of Neutral and basic Substances NH2 Handle aromatic amines with care. Most are toxic and some are carcinogenic. Avoid breathing the dust and vapor from the solid and keep the compounds off the skin, best done by wearing gloves. Naphthalene mp 80°C 4-Chloroaniline mp 68–71°C, pK, 10.0 1) Dissolve 2g of mixture in 20 mL of ethyl ether, and transfer the mixture to a 125 mL separatory funnel. 2) Add 10 mL of H,O and 10 mL of a 3M HCl solution into the funnel. 3) Stopper the funnel, shakes the mixture thoroughly with frequent venting of the funnel. 4) Allow the layers to separate completely, then draw off the lower layer into a 50 mL flask (flask 1) 5) Repeat the process with another 10 mL of HCl. Draw off the lower layer into flask 1. Correct positions for holding a separatory funnel when shaking. FIG. 3

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Create a detailed flow sheet for the following experiment.
**Procedure for Separation and Analysis of Compounds**

6) Add 15 mL of a saturated NaCl solution to a separatory funnel. Shake the funnel and allow the layers to separate. Draw off the lower layer. Carefully pour the ether layer into a 50 mL flask (referred to as flask 2). Add about 4g of anhydrous CaCl₂ and set it aside.

7) Add NaOH dropwise into flask 1 until no more solid is produced. Cool the flask using an ice bath.

8) Decant the ether layer from flask 2 into a new beaker, ensuring that all solid is left behind. Then, evaporate the solution.

9) Collect the solid from flask 1 using suction filtration.

10) Weigh the two compounds and test their melting points (m.p.).

**Figure Explanation**
- The diagram shows a separatory funnel with a Teflon stopcock. Below it is a stand supporting the funnel, which is being used to separate liquids based on their densities. The bottom layer can be drawn off by opening the stopcock, allowing for precise separation of the different phases.
Transcribed Image Text:**Procedure for Separation and Analysis of Compounds** 6) Add 15 mL of a saturated NaCl solution to a separatory funnel. Shake the funnel and allow the layers to separate. Draw off the lower layer. Carefully pour the ether layer into a 50 mL flask (referred to as flask 2). Add about 4g of anhydrous CaCl₂ and set it aside. 7) Add NaOH dropwise into flask 1 until no more solid is produced. Cool the flask using an ice bath. 8) Decant the ether layer from flask 2 into a new beaker, ensuring that all solid is left behind. Then, evaporate the solution. 9) Collect the solid from flask 1 using suction filtration. 10) Weigh the two compounds and test their melting points (m.p.). **Figure Explanation** - The diagram shows a separatory funnel with a Teflon stopcock. Below it is a stand supporting the funnel, which is being used to separate liquids based on their densities. The bottom layer can be drawn off by opening the stopcock, allowing for precise separation of the different phases.
## Extraction (Part 2)

### Experiment: Separation of Neutral and Basic Substances

#### Chemical Structures and Properties:
- **Naphthalene**: Molecular structure with a melting point (mp) of 80°C.
- **4-Chloroaniline**: Molecular structure with melting point (mp) 68-71°C and pKa 10.0.

#### Safety Precautions:
- **Warning**: Handle aromatic amines with care. Most are toxic and some are carcinogenic. Avoid breathing dust and vapors. Keep compounds off the skin, best managed by wearing gloves.

#### Procedure:
1. Dissolve 2g of the mixture in 20 mL of ethyl ether and transfer the mixture to a 125 mL separatory funnel.
2. Add 10 mL of H₂O and 10 mL of a 3M HCl solution into the funnel.
3. Stopper the funnel and shake the mixture thoroughly, frequently venting the funnel.
4. Allow layers to separate completely. Draw off the lower layer into a 50 mL flask (flask 1).
5. Repeat the process with another 10 mL of HCl. Draw off the lower layer into flask 1.

#### Diagram:
- **Figure 3**: Illustration of the correct position for holding a separatory funnel when shaking. This guides safe and effective mixing and separation of substances.

This procedure outlines how to safely and efficiently separate neutral and basic substances for further analysis or experiments.
Transcribed Image Text:## Extraction (Part 2) ### Experiment: Separation of Neutral and Basic Substances #### Chemical Structures and Properties: - **Naphthalene**: Molecular structure with a melting point (mp) of 80°C. - **4-Chloroaniline**: Molecular structure with melting point (mp) 68-71°C and pKa 10.0. #### Safety Precautions: - **Warning**: Handle aromatic amines with care. Most are toxic and some are carcinogenic. Avoid breathing dust and vapors. Keep compounds off the skin, best managed by wearing gloves. #### Procedure: 1. Dissolve 2g of the mixture in 20 mL of ethyl ether and transfer the mixture to a 125 mL separatory funnel. 2. Add 10 mL of H₂O and 10 mL of a 3M HCl solution into the funnel. 3. Stopper the funnel and shake the mixture thoroughly, frequently venting the funnel. 4. Allow layers to separate completely. Draw off the lower layer into a 50 mL flask (flask 1). 5. Repeat the process with another 10 mL of HCl. Draw off the lower layer into flask 1. #### Diagram: - **Figure 3**: Illustration of the correct position for holding a separatory funnel when shaking. This guides safe and effective mixing and separation of substances. This procedure outlines how to safely and efficiently separate neutral and basic substances for further analysis or experiments.
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