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Chem 232 Liquid Liquid Extraction of P-Bromoanaline

Essay by   •  February 24, 2016  •  Lab Report  •  1,001 Words (5 Pages)  •  898 Views

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Chemistry 232     Fall 2015 and Spring 2016

Separation by Chemical Extraction

Abstract

p-Bromoanaline was isolated via liquid-liquid extraction. Phenanthrene was separated and purified via recrystallization. The purity of the phenanthrene sample was determined using the thin layer chromatography method and via the comparison of melting ranges. The % recovery of the crystal phenanthrene was determined to be 110%, and p-bromoanaline was 28 %.

Equation of Extraction and Regeneration

Procedure Reference

Appendix, pages A-2 (Melting Point), A-14 (Rotary Evaporator), A-14 (Recrystallization), A-19 (Extraction), A-24 (Column and Thin-Layer Chromatography)

Liquid-liquid Extraction

Reagents for Extraction

Compound

MW (g/mol)

Used

moles

Physical and Safety Data

p-Bromoanaline

172.03

1.00 g

5.81 x 10-3 mols

Irritant in case of skin/eye contact, hazardous in case of ingestion/inhalations.

MP= 66 C; BP= decomposes

Hydrochloric Acid (HCl)

36.46

3 x 30 mL

0.396 mols

Highly toxic, corrosive (3M solutions). Dispose as aqueous waste.

Density= 1.20 g/M

Phenantherene*

178.23

2.00 g

1.12 x 10-2 mols

Toxic, hazard to aqueous environment.

MP= 98-100 C;  BP= 340 C; density= 1.063 g/M

Dichloromethane

(DCM)

84.93

100 mL

1.56 mols

Toxic, dispose in halogen waste.

BP= 39 C, d= 1.3255 g/mL

Anhydrous Sodium Sulfate

142.04

6.209 g

4.37 x 10-2 mols

Irritant, hydroscopic.

MP= 884 C, d=2.68 g/mL

Sodium Hydroxide

40.00

30 mL

1.59 mols

Toxic, corrosive; 3 M. Dispose in basic aqueous d= 2.13 g/mL

*Phenanthrene remained in the organic layer

Recrystallization of Phenanthrene

Compound

MW (g/mol)

Used

moles

Physical and Safety Data

Phenanthrene

178.23

1.0 g

0.0056 mols

Toxic, hazardous to aqueous environment. Harmful if swallowed

MP= 99-101 C, BP= 346 C, d= 1.063 g/mL

Ethanol

46.07

20 mL

0.340 mols

Flammable liquid, irritant. Dispose as non-halogenated waste. BP= 78 C, d= 0.790 g/mL.

Water

18.02

0.271 g

1.50 x 10-2 mols

Can be hazardous depending on contents. MP= 0C, BP= 100 C; d= 1.00 g/mL

All Products; Crude and Recrystallized

Compound

MW (g/mol)

Isolated

moles

% recovery

Crude phenanthrene

178.20

1.059 g

5.94 x  10-3 mols

53%

Recrystallized Phenanthrene

178.23

1.101 g

6.18 x  10-3 mols

110%

Aqueous precipitate (p-bromoanaline salt)

172.03

0.271 g

1.57 x  10-3 mols

28%

Physical Description

Crude phenanthrene- thick/dense consistency, off-white, powdered solid.

Aqueous precipitate (p-bromoanaline salt)- whitish colour. Crystalized once cooled. Sweetish odour.

Crystallized phenanthrene- original state was thick/dense off-white powdered solid, when hot water added became hard, shiny/sparkly crystals.

Yield Calculation for p-Bromoanaline

% yield = moles of product / moles of start material x 100%

        =  0.001575306 mol / 0.0056 mol

        = 28 % recovery

Yield Calculation for Recrystallization of Phenanthrene

% yield = 0.006178451 mol / 0.0056 mol x 100%

         = 110 % recovery

Melting Range Data

Sample Determined

Observed Melting Range

Lit. Melting Range

Identification

Component from solution A

55°C

60-64°C

p-Bromoanaline

Component from solution B

90 -93°C

111-113°C

m-Toluic Acid

Crude phenanthrene

77-87°C

98-101°C

---

Recrystallized phenanthrene

74-85°C

98-101°C

---

The sample for the melting range of the m-Toluic Acid was supplied by Maddy Wrazej.

Solubility Data

Solubility

Compound

Ethanol

Hexanes

Toluene

Water

cold

hot

cold

hot

cold

hot

cold

Hot

Anthranilic acid

s

V

i

𝛿

i

V

𝛿

s

Phenanthrene

𝛿

s

s

V

V

V

i

i

m-Toluic acid

𝛿

V

s

V

V

V

i

i

p-Bromoaniline

𝛿

s

𝛿

V

s

V

i

𝛿

...

...

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